#------------------------------------------------------------------------------
#$Date: 2025-08-19 16:18:28 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/22/41/2224124.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2224124
loop_
_publ_author_name
'Takahashi, Yuya'
'Ikeda, Yasuhisa'
_publ_section_title
;
 trans-Bis(1-cyclohexylpyrrolidin-2-one)dinitratopalladium(II)
;
_journal_coeditor_code           BR2124
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1533
_journal_page_last               m1534
_journal_paper_doi               10.1107/S1600536809045930
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pd (N O3)2 (C10 H17 N O)2]'
_chemical_formula_moiety         'C20 H34 N4 O8 Pd1'
_chemical_formula_sum            'C20 H34 N4 O8 Pd'
_chemical_formula_weight         564.91
_chemical_name_systematic
;
trans-Bis(1-cyclohexylpyrrolidin-2-one)dinitratopalladium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                60.8650(19)
_cell_angle_beta                 66.057(2)
_cell_angle_gamma                68.845(2)
_cell_formula_units_Z            1
_cell_length_a                   7.6431(5)
_cell_length_b                   9.8892(8)
_cell_length_c                   10.1118(7)
_cell_measurement_reflns_used    5845
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     597.24(8)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1994) and DIRDIF99 (Beurskens et
al.,
1999)
;
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5836
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1999)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             292.00
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2696
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0294P)²+0.1351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0518
_reflns_number_gt                2662
_reflns_number_total             2696
_reflns_threshold_expression     F²>2σ(F²)
_cod_data_source_file            br2124.cif
_cod_data_source_block           I
_cod_original_cell_volume        597.24(7)
_cod_original_formula_sum        'C20 H34 N4 O8 Pd1'
_cod_database_code               2224124
_cod_database_fobs_code          2224124
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd(1) 1.0000 1.0000 0.0000 0.02155(5) Uani d S 1.00 . .
O O(1) 0.92669(15) 0.93354(13) 0.23446(12) 0.0268(2) Uani d . 1.00 . .
O O(2) 1.18410(17) 1.12278(13) -0.03171(13) 0.0308(2) Uani d . 1.00 . .
O O(3) 0.98979(19) 1.33981(14) -0.14453(18) 0.0454(3) Uani d . 1.00 . .
O O(4) 1.25913(19) 1.34980(16) -0.12849(17) 0.0447(3) Uani d . 1.00 . .
N N(1) 1.14168(19) 1.27768(16) -0.10479(15) 0.0289(2) Uani d . 1.00 . .
N N(2) 0.99744(17) 0.78446(13) 0.46810(13) 0.0201(2) Uani d . 1.00 . .
C C(1) 1.04947(19) 0.84244(15) 0.31243(15) 0.0200(2) Uani d . 1.00 . .
C C(2) 1.2637(2) 0.78476(17) 0.24741(16) 0.0246(2) Uani d . 1.00 . .
C C(3) 1.3405(2) 0.70029(19) 0.39282(17) 0.0283(3) Uani d . 1.00 . .
C C(4) 1.1591(2) 0.6721(2) 0.53523(17) 0.0308(3) Uani d . 1.00 . .
C C(5) 0.79357(19) 0.80910(15) 0.56480(15) 0.0197(2) Uani d . 1.00 . .
C C(6) 0.7016(2) 0.67022(18) 0.61976(19) 0.0284(3) Uani d . 1.00 . .
C C(7) 0.4882(2) 0.6965(2) 0.7192(2) 0.0320(3) Uani d . 1.00 . .
C C(8) 0.4713(2) 0.7307(2) 0.85611(18) 0.0331(3) Uani d . 1.00 . .
C C(9) 0.5632(2) 0.8697(2) 0.79808(19) 0.0329(3) Uani d . 1.00 . .
C C(10) 0.7782(2) 0.8389(2) 0.70401(18) 0.0288(3) Uani d . 1.00 . .
H H(1) 1.4309 0.5987 0.3943 0.034 Uiso c R 1.00 . .
H H(2) 1.4106 0.7671 0.3930 0.034 Uiso c R 1.00 . .
H H(3) 0.7185 0.9056 0.4966 0.024 Uiso c R 1.00 . .
H H(4) 1.1427 0.5617 0.5814 0.037 Uiso c R 1.00 . .
H H(5) 1.1670 0.6947 0.6176 0.037 Uiso c R 1.00 . .
H H(6) 0.8353 0.9314 0.6650 0.035 Uiso c R 1.00 . .
H H(7) 0.8527 0.7458 0.7733 0.035 Uiso c R 1.00 . .
H H(8) 0.5543 0.8869 0.8894 0.040 Uiso c R 1.00 . .
H H(9) 0.4907 0.9666 0.7304 0.040 Uiso c R 1.00 . .
H H(10) 0.3316 0.7544 0.9134 0.040 Uiso c R 1.00 . .
H H(11) 0.5371 0.6359 0.9307 0.040 Uiso c R 1.00 . .
H H(12) 0.4091 0.7865 0.6515 0.038 Uiso c R 1.00 . .
H H(13) 0.4353 0.6011 0.7612 0.038 Uiso c R 1.00 . .
H H(14) 1.3286 0.8742 0.1665 0.030 Uiso c R 1.00 . .
H H(15) 1.2847 0.7108 0.2003 0.030 Uiso c R 1.00 . .
H H(16) 0.7772 0.5718 0.6833 0.034 Uiso c R 1.00 . .
H H(17) 0.7068 0.6578 0.5268 0.034 Uiso c R 1.00 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.999 1.007
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, 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_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) Pd(1) O(1) . . 2_775 180.00(7) no
O(1) Pd(1) O(2) . . . 89.93(5) no
O(1) Pd(1) O(2) . . 2_775 90.07(5) no
O(1) Pd(1) O(2) 2_775 . . 90.07(5) no
O(1) Pd(1) O(2) 2_775 . 2_775 89.93(5) no
O(2) Pd(1) O(2) . . 2_775 180.00(6) no
Pd(1) O(1) C(1) . . . 121.33(8) no
Pd(1) O(2) N(1) . . . 117.47(11) no
O(2) N(1) O(3) . . . 118.89(17) no
O(2) N(1) O(4) . . . 116.54(14) no
O(3) N(1) O(4) . . . 124.58(13) no
C(1) N(2) C(4) . . . 112.87(10) no
C(1) N(2) C(5) . . . 123.33(12) no
C(4) N(2) C(5) . . . 123.11(10) no
O(1) C(1) N(2) . . . 121.72(11) no
O(1) C(1) C(2) . . . 127.06(11) no
N(2) C(1) C(2) . . . 111.21(11) no
C(1) C(2) C(3) . . . 103.45(11) no
C(2) C(3) C(4) . . . 105.44(12) no
N(2) C(4) C(3) . . . 103.45(10) no
N(2) C(5) C(6) . . . 110.78(12) no
N(2) C(5) C(10) . . . 111.59(14) no
C(6) C(5) C(10) . . . 111.32(11) no
C(5) C(6) C(7) . . . 110.86(14) no
C(6) C(7) C(8) . . . 111.34(17) no
C(7) C(8) C(9) . . . 111.23(12) no
C(8) C(9) C(10) . . . 110.64(16) no
C(5) C(10) C(9) . . . 109.88(17) no
C(1) C(2) H(14) . . . 111.1 no
C(1) C(2) H(15) . . . 111.1 no
C(3) C(2) H(14) . . . 111.1 no
C(3) C(2) H(15) . . . 111.1 no
H(14) C(2) H(15) . . . 109.0 no
C(2) C(3) H(1) . . . 110.7 no
C(2) C(3) H(2) . . . 110.7 no
C(4) C(3) H(1) . . . 110.7 no
C(4) C(3) H(2) . . . 110.7 no
H(1) C(3) H(2) . . . 108.8 no
N(2) C(4) H(4) . . . 111.1 no
N(2) C(4) H(5) . . . 111.1 no
C(3) C(4) H(4) . . . 111.1 no
C(3) C(4) H(5) . . . 111.1 no
H(4) C(4) H(5) . . . 109.0 no
N(2) C(5) H(3) . . . 107.6 no
C(6) C(5) H(3) . . . 107.7 no
C(10) C(5) H(3) . . . 107.6 no
C(5) C(6) H(16) . . . 109.5 no
C(5) C(6) H(17) . . . 109.5 no
C(7) C(6) H(16) . . . 109.5 no
C(7) C(6) H(17) . . . 109.5 no
H(16) C(6) H(17) . . . 108.1 no
C(6) C(7) H(12) . . . 109.4 no
C(6) C(7) H(13) . . . 109.4 no
C(8) C(7) H(12) . . . 109.4 no
C(8) C(7) H(13) . . . 109.4 no
H(12) C(7) H(13) . . . 108.0 no
C(7) C(8) H(10) . . . 109.4 no
C(7) C(8) H(11) . . . 109.4 no
C(9) C(8) H(10) . . . 109.4 no
C(9) C(8) H(11) . . . 109.4 no
H(10) C(8) H(11) . . . 108.0 no
C(8) C(9) H(8) . . . 109.5 no
C(8) C(9) H(9) . . . 109.5 no
C(10) C(9) H(8) . . . 109.5 no
C(10) C(9) H(9) . . . 109.5 no
H(8) C(9) H(9) . . . 108.1 no
C(5) C(10) H(6) . . . 109.7 no
C(5) C(10) H(7) . . . 109.7 no
C(9) C(10) H(6) . . . 109.7 no
C(9) C(10) H(7) . . . 109.7 no
H(6) C(10) H(7) . . . 108.2 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd(1) O(1) . . 2.0092(11) yes
Pd(1) O(1) . 2_775 2.0092(11) no
Pd(1) O(2) . . 2.0112(15) yes
Pd(1) O(2) . 2_775 2.0112(15) no
O(1) C(1) . . 1.2699(17) no
O(2) N(1) . . 1.3158(16) no
O(3) N(1) . . 1.229(2) no
O(4) N(1) . . 1.222(2) no
N(2) C(1) . . 1.3200(17) no
N(2) C(4) . . 1.4754(19) no
N(2) C(5) . . 1.4713(15) no
C(1) C(2) . . 1.5020(17) no
C(2) C(3) . . 1.535(2) no
C(3) C(4) . . 1.5304(18) no
C(5) C(6) . . 1.525(2) no
C(5) C(10) . . 1.525(2) no
C(6) C(7) . . 1.5351(19) no
C(7) C(8) . . 1.525(3) no
C(8) C(9) . . 1.518(3) no
C(9) C(10) . . 1.533(2) no
C(2) H(14) . . 0.990 no
C(2) H(15) . . 0.990 no
C(3) H(1) . . 0.990 no
C(3) H(2) . . 0.990 no
C(4) H(4) . . 0.990 no
C(4) H(5) . . 0.990 no
C(5) H(3) . . 1.000 no
C(6) H(16) . . 0.990 no
C(6) H(17) . . 0.990 no
C(7) H(12) . . 0.990 no
C(7) H(13) . . 0.990 no
C(8) H(10) . . 0.990 no
C(8) H(11) . . 0.990 no
C(9) H(8) . . 0.990 no
C(9) H(9) . . 0.990 no
C(10) H(6) . . 0.990 no
C(10) H(7) . . 0.990 no
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O(1) Pd(1) O(2) N(1) . . . . -113.91(10) ?
O(2) Pd(1) O(1) C(1) . . . . -66.76(14) ?
O(1) Pd(1) O(2) N(1) . . 2_775 2_775 -66.09(10) ?
O(2) Pd(1) O(1) C(1) 2_775 . . . 113.24(14) ?
O(1) Pd(1) O(2) N(1) 2_775 . . . 66.09(10) ?
O(2) Pd(1) O(1) C(1) . . 2_775 2_775 -113.24(14) ?
O(1) Pd(1) O(2) N(1) 2_775 . 2_775 2_775 113.91(10) ?
O(2) Pd(1) O(1) C(1) 2_775 . 2_775 2_775 66.76(14) ?
Pd(1) O(1) C(1) N(2) . . . . -172.54(13) ?
Pd(1) O(1) C(1) C(2) . . . . 6.7(2) ?
Pd(1) O(2) N(1) O(3) . . . . 2.66(19) ?
Pd(1) O(2) N(1) O(4) . . . . -177.21(12) ?
C(1) N(2) C(4) C(3) . . . . 14.4(2) ?
C(4) N(2) C(1) O(1) . . . . 175.65(17) ?
C(4) N(2) C(1) C(2) . . . . -3.7(2) ?
C(1) N(2) C(5) C(6) . . . . 95.31(17) ?
C(1) N(2) C(5) C(10) . . . . -140.05(16) ?
C(5) N(2) C(1) O(1) . . . . 4.9(2) ?
C(5) N(2) C(1) C(2) . . . . -174.43(15) ?
C(4) N(2) C(5) C(6) . . . . -74.5(2) ?
C(4) N(2) C(5) C(10) . . . . 50.2(2) ?
C(5) N(2) C(4) C(3) . . . . -174.89(17) ?
O(1) C(1) C(2) C(3) . . . . 172.09(18) ?
N(2) C(1) C(2) C(3) . . . . -8.6(2) ?
C(1) C(2) C(3) C(4) . . . . 16.71(19) ?
C(2) C(3) C(4) N(2) . . . . -18.6(2) ?
N(2) C(5) C(6) C(7) . . . . -179.40(13) ?
N(2) C(5) C(10) C(9) . . . . 178.01(11) ?
C(6) C(5) C(10) C(9) . . . . -57.65(14) ?
C(10) C(5) C(6) C(7) . . . . 55.81(17) ?
C(5) C(6) C(7) C(8) . . . . -54.16(16) ?
C(6) C(7) C(8) C(9) . . . . 55.18(16) ?
C(7) C(8) C(9) C(10) . . . . -57.20(18) ?
C(8) C(9) C(10) C(5) . . . . 58.08(16) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139077811
