Palladium(ii) complexes of tetradentate donor‒acceptor Schiff base ligands: synthesis and spectral, structural, thermal and NLO properties
Celedón, Salvador; Roisnel, Thierry; Artigas, Vania; Fuentealba, Mauricio; Carrillo, David; Ledoux-Rak, Isabelle; Hamon, Jean-René; Manzur, Carolina; New Journal of Chemistry 44 (2020) 9190–9201; doi:10.1039/D0NJ01982H

data_7059607
_publ_section_title
;
 Palladium(ii) complexes of tetradentate donor--acceptor Schiff base
 ligands: synthesis and spectral, structural, thermal and NLO properties
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9190
_journal_page_last               9201
_journal_paper_doi               10.1039/D0NJ01982H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C38 H39 Fe N2 O3 Pd Ru, F6 P'
_chemical_formula_sum            'C38 H39 F6 Fe N2 O3 P Pd Ru'
_chemical_formula_weight         980.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2768(4)
_cell_length_b                   17.7955(5)
_cell_length_c                   16.8416(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.42
_cell_volume                     3673.84(19)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         2.017
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0648 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.8488.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0488P)^2^+13.8034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5443
_reflns_number_total             7433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01982h2.cif
_cod_data_source_block           testa
_cod_depositor_comments
;Adding full bibliography for 7059607--7059608.cif.

 Adding full bibliography for 7059607--7059608.cif.
;
_cod_database_code               7059607
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.664
_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, All O(H) groups
2. Restrained distances
 F3-F4 \\sim F3-F6 \\sim F3-F1 \\sim F3-F2 \\sim F1A-F5A \\sim F1A-F4A \\sim
F1A-F2A \\sim F1A-F3A \\sim F5A-
 F6A \\sim F5A-F4A \\sim F5A-F2A \\sim F4-F6 \\sim F4-F5 \\sim F4-F1 \\sim
F6A-F4A \\sim F6A-F2A \\sim F6A-F3A
 \\sim F6-F5 \\sim F6-F2 \\sim F4A-F3A \\sim F2A-F3A \\sim F5-F1 \\sim F5-F2
\\sim F1-F2
 with sigma of 0.04
 P1-F3 \\sim P1-F1A \\sim P1-F5A \\sim P1-F4 \\sim P1-F6A \\sim P1-F6 \\sim
P1-F4A \\sim P1-F2A \\sim P1-F5 ~
 P1-F1 \\sim P1-F2 \\sim P1-F3A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C3-C2 \\sim C3A-C2A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 C1-C5 \\sim C1A-C5A
 with sigma of 0.02
 Fe1-C4 \\sim Fe1-C4A
 with sigma of 0.04
 Fe1-C3 \\sim Fe1-C3A
 with sigma of 0.04
 Fe1-C2 \\sim Fe1-C2A
 with sigma of 0.04
 Fe1-C1 \\sim Fe1-C1A
 with sigma of 0.04
 Fe1-C5 \\sim Fe1-C5A
 with sigma of 0.04
 C4-C2 \\sim C4A-C2A
 with sigma of 0.04
 C4-C1 \\sim C4A-C1A
 with sigma of 0.04
 C3-C1 \\sim C3A-C1A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C2-C5 \\sim C2A-C5A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F4A)
Uanis(F5) = Uanis(F5A)
Uanis(F6) = Uanis(F6A)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C5)
4. Others
 Sof(F3A)=Sof(F6A)=Sof(F4A)=Sof(F1A)=Sof(F2A)=Sof(F5A)=1-FVAR(1)
 Sof(F2)=Sof(F1)=Sof(F4)=Sof(F5)=Sof(F3)=Sof(F6)=FVAR(1)
 Fixed Sof: C4(0.5) H4(0.5) C3(0.5) H3A(0.5) C2(0.5) H2(0.5) C1(0.5) H1(0.5)
 C5(0.5) H5(0.5) C3A(0.5) H3AA(0.5) C2A(0.5) H2A(0.5) C1A(0.5) H1A(0.5)
 C5A(0.5) H5A(0.5) C4A(0.5) H4A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C26(H26), C24(H24), C25(H25), C22(H22), C15(H15), C6(H6), C18(H18),
 C19(H19), C9(H9), C12(H12), C16(H16), C7(H7), C8(H8), C4(H4), C3(H3A), C2(H2),
 C1(H1), C5(H5), C3A(H3AA), C2A(H2A), C1A(H1A), C5A(H5A), C4A(H4A)
5.c Fitted pentagon refined as free rotating group:
 C4(C3,C2,C1,C5)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C35(H35A,H35B,
 H35C), C34(H34A,H34B,H34C)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'