Mechanochemistry for the synthesis of non-classical N-metalated palladium(ii) pincer complexes
Aleksanyan, Diana V.; Churusova, Svetlana G.; Brunova, Valentina V.; Peregudov, Alexander S.; Shakhov, Aleksander M.; Rybalkina, Ekaterina Yu.; Klemenkova, Zinaida S.; Kononova, Elena G.; Denisov, Gleb L.; Kozlov, Vladimir A.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03259C

data_7708805
_publ_section_title
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 Mechanochemistry for the synthesis of non-classical N-metalated
 palladium(ii) pincer complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03259C
_journal_year                    2021
_chemical_formula_moiety         'C19 H16 Cl N3 O2 Pd S2, C H2 Cl2'
_chemical_formula_sum            'C20 H18 Cl3 N3 O2 Pd S2'
_chemical_formula_weight         609.24
_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             2020-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2020-04-26 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.8300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1861(11)
_cell_length_b                   12.4176(10)
_cell_length_c                   13.8527(11)
_cell_measurement_reflns_used    4293
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.30
_cell_volume                     2177.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.8294.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4078
_reflns_number_total             5265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03259c2.cif
_cod_data_source_block           12
_cod_database_code               7708805
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'