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#$Date: 2024-09-06 03:40:52 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294548 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/67/7716792.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_7716792
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+), (C7 H11 O3 1-)2'
_chemical_formula_sum            'C14 H22 O6 Pd'
_chemical_formula_weight         392.71
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2024-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.35329(10)
_cell_length_b                   10.3794(3)
_cell_length_c                   17.7657(5)
_cell_measurement_reflns_used    2993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.7010
_cell_measurement_theta_min      4.9360
_cell_volume                     801.33(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov, 2009)'
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'Olex2 1.3 (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.977
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5007
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         4.937
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.558
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    1.628
_exptl_crystal_description       needle
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0346
_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)+(0.0641P)²+0.1273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1404
_reflns_number_total             1605
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01287a3.cif
_cod_data_source_block           nab22-3Dshape
_cod_depositor_comments
'Adding full bibliography for 7716790--7716792.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716792
_shelx_shelxl_version_number     2018/1
_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_min   0.370
_shelx_estimated_absorpt_t_max   0.832
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.000000 0.500000 0.500000 0.02524(16) Uani 1 2 d S . P . .
C1 C 0.5896(8) 0.8236(3) 0.48580(17) 0.0347(6) Uani 1 1 d . . . . .
H1A H 0.748542 0.793745 0.453077 0.052 Uiso 1 1 calc R U . . .
H1B H 0.684515 0.876674 0.526457 0.052 Uiso 1 1 calc R U . . .
H1C H 0.436973 0.874896 0.456183 0.052 Uiso 1 1 calc R U . . .
O1 O 0.2373(4) 0.65426(19) 0.47275(10) 0.0295(4) Uani 1 1 d . . . . .
C2 C 0.4342(6) 0.7092(3) 0.51911(16) 0.0279(5) Uani 1 1 d . . . . .
C3 C 0.5119(6) 0.6739(3) 0.59272(15) 0.0302(6) Uani 1 1 d . . . . .
H3 H 0.657782 0.725966 0.620529 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3920(6) 0.5665(3) 0.62994(14) 0.0274(5) Uani 1 1 d . . . . .
O4 O 0.1892(7) 0.48881(18) 0.60510(16) 0.0293(5) Uani 1 1 d . . . . .
O5 O 0.5123(4) 0.5498(2) 0.70038(10) 0.0303(4) Uani 1 1 d . . . . .
C5 C 0.3809(7) 0.4485(3) 0.74587(16) 0.0327(6) Uani 1 1 d . . . . .
H5 H 0.151699 0.448719 0.737435 0.039 Uiso 1 1 calc R U . . .
C6 C 0.4686(11) 0.4859(3) 0.8269(2) 0.0386(9) Uani 1 1 d . . . . .
H6A H 0.693189 0.485577 0.835117 0.058 Uiso 1 1 calc R U . . .
H6B H 0.379431 0.424044 0.861092 0.058 Uiso 1 1 calc R U . . .
H6C H 0.389817 0.572365 0.836771 0.058 Uiso 1 1 calc R U . . .
C7 C 0.5050(7) 0.3179(3) 0.72557(17) 0.0388(7) Uani 1 1 d . . . . .
H7A H 0.461051 0.301883 0.671638 0.058 Uiso 1 1 calc R U . . .
H7B H 0.406494 0.251143 0.754857 0.058 Uiso 1 1 calc R U . . .
H7C H 0.727908 0.315829 0.737047 0.058 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
O1 Pd1 O1 180.00(9) 3_566 . ?
O1 Pd1 O4 85.23(8) 3_566 . ?
O1 Pd1 O4 94.77(8) . . ?
O1 Pd1 O4 94.78(8) 3_566 3_566 ?
O1 Pd1 O4 85.22(8) . 3_566 ?
O4 Pd1 O4 180.0 . 3_566 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 O1 Pd1 122.62(18) . . ?
O1 C2 C3 127.3(3) . . ?
O1 C2 C1 113.3(2) . . ?
C3 C2 C1 119.4(2) . . ?
C2 C3 C4 125.2(2) . . ?
C2 C3 H3 117.4 . . ?
C4 C3 H3 117.4 . . ?
O4 C4 O5 118.2(2) . . ?
O4 C4 C3 127.9(2) . . ?
O5 C4 C3 113.9(2) . . ?
C4 O4 Pd1 122.20(19) . . ?
C4 O5 C5 117.7(2) . . ?
O5 C5 C7 110.9(2) . . ?
O5 C5 C6 104.8(3) . . ?
C7 C5 C6 112.5(3) . . ?
O5 C5 H5 109.5 . . ?
C7 C5 H5 109.5 . . ?
C6 C5 H5 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 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 O1 1.9811(19) 3_566 ?
Pd1 O1 1.9811(19) . ?
Pd1 O4 1.999(3) . ?
Pd1 O4 1.999(3) 3_566 ?
C1 C2 1.505(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O1 C2 1.286(3) . ?
C2 C3 1.381(4) . ?
C3 C4 1.411(4) . ?
C3 H3 0.9500 . ?
C4 O4 1.256(4) . ?
C4 O5 1.339(3) . ?
O5 C5 1.463(4) . ?
C5 C7 1.511(4) . ?
C5 C6 1.518(5) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 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 O1 C2 C3 -0.5(4) . . . . ?
Pd1 O1 C2 C1 179.24(19) . . . . ?
O1 C2 C3 C4 1.9(5) . . . . ?
C1 C2 C3 C4 -177.8(3) . . . . ?
C2 C3 C4 O4 -3.2(5) . . . . ?
C2 C3 C4 O5 177.6(3) . . . . ?
O5 C4 O4 Pd1 -178.20(17) . . . . ?
C3 C4 O4 Pd1 2.7(4) . . . . ?
O4 C4 O5 C5 -5.0(4) . . . . ?
C3 C4 O5 C5 174.2(2) . . . . ?
C4 O5 C5 C7 79.8(3) . . . . ?
C4 O5 C5 C6 -158.6(3) . . . . ?
