#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:40:52 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294548 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/67/7716791.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716791
loop_
_publ_author_name
'Butrymowicz-Kubiak, A'
'Muzioł, T M'
'Kaczmarek-Kędziera, A'
'Jureddy, C. S.'
'Maćkosz, K'
'Utke, I.'
'Szymańska, I B'
_publ_section_title
;
 New palladium(II) β-ketoesterates for focused electron beam induced
 deposition: synthesis, structures, and characterization.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13662
_journal_page_last               13677
_journal_paper_doi               10.1039/d4dt01287a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '(Pd 2+), (C6 H9 O3 1-)2'
_chemical_formula_sum            'C12 H18 O6 Pd'
_chemical_formula_weight         364.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-07
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2024-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                89.994(3)
_cell_angle_beta                 80.180(3)
_cell_angle_gamma                79.606(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0247(2)
_cell_length_b                   8.6043(3)
_cell_length_c                   11.5706(4)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      5.2120
_cell_measurement_theta_min      78.0190
_cell_volume                     677.46(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8513
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.475
_diffrn_reflns_theta_min         3.879
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.252
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0261
_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/[σ²(Fo²)+(0.0513P)²+0.1198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2451
_reflns_number_total             2756
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01287a3.cif
_cod_data_source_block           nab20-3dshape
_cod_depositor_comments
'Adding full bibliography for 7716790--7716792.cif.'
_cod_database_code               7716791
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.399
_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 Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.500000 0.500000 0.500000 0.01756(10) Uani 1 2 d S . P . .
C1 C 0.8212(4) -0.1723(3) 0.6195(2) 0.0252(5) Uani 1 1 d . . . . .
H1A H 0.955117 -0.218700 0.581729 0.038 Uiso 1 1 calc R U . . .
H1B H 0.728667 -0.234204 0.596584 0.038 Uiso 1 1 calc R U . . .
H1C H 0.812576 -0.173014 0.704952 0.038 Uiso 1 1 calc R U . . .
C2 C 0.7705(3) -0.0041(3) 0.5815(2) 0.0226(5) Uani 1 1 d . . . . .
H2A H 0.859842 0.060819 0.606702 0.027 Uiso 1 1 calc R U . . .
H2B H 0.783396 -0.001244 0.495002 0.027 Uiso 1 1 calc R U . . .
C3 C 0.4883(3) 0.2023(3) 0.6106(2) 0.0206(4) Uani 1 1 d . . . . .
O3 O 0.5684(2) 0.05648(18) 0.63665(15) 0.0229(3) Uani 1 1 d . . . . .
O3A O 0.5972(2) 0.27993(17) 0.54442(14) 0.0214(3) Uani 1 1 d . . . . .
C4 C 0.2900(4) 0.2491(3) 0.6610(2) 0.0215(4) Uani 1 1 d . . . . .
H4 H 0.231693 0.178158 0.712560 0.026 Uiso 1 1 calc R U . . .
O5 O 0.2255(2) 0.50454(18) 0.57950(14) 0.0214(3) Uani 1 1 d . . . . .
C5 C 0.1722(4) 0.3908(3) 0.6416(2) 0.0203(5) Uani 1 1 d . . . . .
C6 C -0.0424(3) 0.4209(3) 0.6937(2) 0.0238(5) Uani 1 1 d . . . . .
H6A H -0.076950 0.522982 0.736680 0.036 Uiso 1 1 calc R U . . .
H6B H -0.070230 0.336727 0.747559 0.036 Uiso 1 1 calc R U . . .
H6C H -0.120140 0.422552 0.630806 0.036 Uiso 1 1 calc R U . . .
Pd2 Pd 0.000000 0.500000 1.000000 0.01774(10) Uani 1 2 d S . P . .
C11 C 0.7950(3) 0.0669(3) 0.9039(2) 0.0254(5) Uani 1 1 d . . . . .
H11A H 0.842229 0.057682 0.819034 0.038 Uiso 1 1 calc R U . . .
H11B H 0.805384 -0.038852 0.936485 0.038 Uiso 1 1 calc R U . . .
H11C H 0.874851 0.127942 0.940733 0.038 Uiso 1 1 calc R U . . .
C12 C 0.5831(4) 0.1499(3) 0.9278(2) 0.0235(4) Uani 1 1 d . . . . .
H12A H 0.500203 0.088582 0.892108 0.028 Uiso 1 1 calc R U . . .
H12B H 0.533940 0.161555 1.013333 0.028 Uiso 1 1 calc R U . . .
C13 C 0.4063(3) 0.4048(3) 0.8963(2) 0.0213(4) Uani 1 1 d . . . . .
O13A O 0.2624(2) 0.36019(17) 0.96029(14) 0.0220(3) Uani 1 1 d . . . . .
O13 O 0.5770(2) 0.30415(18) 0.87596(15) 0.0222(3) Uani 1 1 d . . . . .
C14 C 0.4101(4) 0.5499(3) 0.8412(2) 0.0224(5) Uani 1 1 d . . . . .
H14 H 0.532982 0.567089 0.799710 0.027 Uiso 1 1 calc R U . . .
C15 C 0.2498(4) 0.6696(3) 0.8424(2) 0.0221(5) Uani 1 1 d . . . . .
O15 O 0.0737(2) 0.67278(18) 0.89751(14) 0.0217(3) Uani 1 1 d . . . . .
C16 C 0.2735(3) 0.8145(3) 0.7718(2) 0.0261(5) Uani 1 1 d . . . . .
H16A H 0.214118 0.810493 0.701406 0.039 Uiso 1 1 calc R U . . .
H16B H 0.413599 0.817623 0.748792 0.039 Uiso 1 1 calc R U . . .
H16C H 0.208208 0.909446 0.819474 0.039 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3A Pd1 O3A 180.0 2_666 . ?
O5 Pd1 O3A 85.40(6) 2_666 . ?
O5 Pd1 O3A 94.60(6) 2_666 2_666 ?
O5 Pd1 O3A 85.40(6) . 2_666 ?
O5 Pd1 O3A 94.60(6) . . ?
O5 Pd1 O5 180.0 2_666 . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
O3 C2 C1 106.99(19) . . ?
O3 C2 H2A 110.3 . . ?
O3 C2 H2B 110.3 . . ?
O3 C3 C4 114.4(2) . . ?
O3A C3 O3 117.4(2) . . ?
O3A C3 C4 128.2(2) . . ?
C3 O3 C2 117.49(18) . . ?
C3 O3A Pd1 122.01(14) . . ?
C3 C4 H4 117.4 . . ?
C5 C4 C3 125.1(2) . . ?
C5 C4 H4 117.4 . . ?
C5 O5 Pd1 122.94(16) . . ?
C4 C5 C6 119.7(2) . . ?
O5 C5 C4 126.8(2) . . ?
O5 C5 C6 113.5(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O13A Pd2 O13A 180.0 2_567 . ?
O15 Pd2 O13A 94.64(6) . . ?
O15 Pd2 O13A 85.36(6) . 2_567 ?
O15 Pd2 O13A 94.64(6) 2_567 2_567 ?
O15 Pd2 O13A 85.36(6) 2_567 . ?
O15 Pd2 O15 180.0 . 2_567 ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
C11 C12 H12A 110.4 . . ?
C11 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
O13 C12 C11 106.80(19) . . ?
O13 C12 H12A 110.4 . . ?
O13 C12 H12B 110.4 . . ?
O13A C13 O13 117.8(2) . . ?
O13A C13 C14 128.0(2) . . ?
O13 C13 C14 114.2(2) . . ?
C13 O13A Pd2 122.04(14) . . ?
C13 O13 C12 117.30(18) . . ?
C13 C14 H14 117.3 . . ?
C15 C14 C13 125.3(2) . . ?
C15 C14 H14 117.3 . . ?
C14 C15 C16 119.3(2) . . ?
O15 C15 C14 127.0(2) . . ?
O15 C15 C16 113.7(2) . . ?
C15 O15 Pd2 122.60(16) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O3A 1.9923(15) 2_666 ?
Pd1 O3A 1.9923(15) . ?
Pd1 O5 1.9833(15) 2_666 ?
Pd1 O5 1.9833(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.511(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 O3 1.455(3) . ?
C3 O3 1.336(3) . ?
C3 O3A 1.266(3) . ?
C3 C4 1.402(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(4) . ?
O5 C5 1.287(3) . ?
C5 C6 1.501(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Pd2 O13A 1.9917(16) 2_567 ?
Pd2 O13A 1.9917(16) . ?
Pd2 O15 1.9881(15) . ?
Pd2 O15 1.9881(15) 2_567 ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C12 1.509(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 O13 1.453(3) . ?
C13 O13A 1.266(3) . ?
C13 O13 1.332(3) . ?
C13 C14 1.404(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(4) . ?
C15 O15 1.287(3) . ?
C15 C16 1.509(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O5 C5 C4 -1.7(3) . . . . ?
Pd1 O5 C5 C6 179.70(14) . . . . ?
C1 C2 O3 C3 -176.84(19) . . . . ?
C3 C4 C5 O5 -3.3(4) . . . . ?
C3 C4 C5 C6 175.2(2) . . . . ?
O3 C3 O3A Pd1 -178.99(14) . . . . ?
O3 C3 C4 C5 -176.1(2) . . . . ?
O3A C3 O3 C2 -3.4(3) . . . . ?
O3A C3 C4 C5 3.5(4) . . . . ?
C4 C3 O3 C2 176.2(2) . . . . ?
C4 C3 O3A Pd1 1.5(3) . . . . ?
C11 C12 O13 C13 -173.57(19) . . . . ?
C13 C14 C15 O15 3.4(4) . . . . ?
C13 C14 C15 C16 -175.6(2) . . . . ?
O13A C13 O13 C12 0.9(3) . . . . ?
O13A C13 C14 C15 -3.7(4) . . . . ?
O13 C13 O13A Pd2 178.94(14) . . . . ?
O13 C13 C14 C15 175.7(2) . . . . ?
C14 C13 O13A Pd2 -1.7(3) . . . . ?
C14 C13 O13 C12 -178.5(2) . . . . ?
C14 C15 O15 Pd2 2.2(3) . . . . ?
C16 C15 O15 Pd2 -178.75(15) . . . . ?
