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#$Date: 2023-01-13 10:32:10 +0200 (Fri, 13 Jan 2023) $
#$Revision: 280326 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/64/8106460.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_8106460
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Crystal structure of (1,4,8,11-tetraazacyclotetradecane)palladium(II)
 tetracyanopalladate(II), C14H24N8Pd2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              139
_journal_page_last               140
_journal_paper_doi               10.1515/ncrs-2016-0193
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C10 H24 N4 Pd, C4 N4 Pd'
_chemical_formula_sum            'C14 H24 N8 Pd2'
_chemical_formula_weight         517.21
_chemical_name_systematic
; 
(1,4,8,11-Tetraazacyclotetradecane)palladium(II) tetracyanopalladate(II)
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.895(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.075(2)
_cell_length_b                   8.3534(19)
_cell_length_c                   12.106(3)
_cell_measurement_reflns_used    5293
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.70
_cell_volume                     914.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11356
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       Block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0220
_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)+(0.0289P)²+0.1761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1591
_reflns_number_total             2185
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2016-0193_suppl.cif
_cod_data_source_block           No07
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        914.3(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8106460
_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   0.617
_shelx_estimated_absorpt_t_max   0.756
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 0.5000 0.5000 0.0000 0.02365(9) Uani 1 2 d S . P . .
N1 N 0.41976(16) 0.33760(17) -0.11655(12) 0.0334(3) Uani 1 1 d . . . . .
H1 H 0.3186 0.3731 -0.1427 0.040 Uiso 1 1 calc R U . . .
N2 N 0.44116(16) 0.33414(17) 0.11241(11) 0.0319(3) Uani 1 1 d . . . . .
H2 H 0.5324 0.2765 0.1398 0.038 Uiso 1 1 calc R U . . .
C1 C 0.4039(2) 0.1821(2) -0.05828(16) 0.0405(5) Uani 1 1 d . . . . .
H1A H 0.5003 0.1292 -0.0461 0.049 Uiso 1 1 calc R U . . .
H1B H 0.3367 0.1114 -0.1032 0.049 Uiso 1 1 calc R U . . .
C2 C 0.3427(2) 0.2161(2) 0.05134(16) 0.0391(4) Uani 1 1 d . . . . .
H2A H 0.2422 0.2594 0.0390 0.047 Uiso 1 1 calc R U . . .
H2B H 0.3386 0.1172 0.0945 0.047 Uiso 1 1 calc R U . . .
C3 C 0.3758(2) 0.4014(2) 0.21109(15) 0.0400(5) Uani 1 1 d . . . . .
H3A H 0.3531 0.3138 0.2607 0.048 Uiso 1 1 calc R U . . .
H3B H 0.2829 0.4559 0.1871 0.048 Uiso 1 1 calc R U . . .
C4 C 0.4792(3) 0.5185(2) 0.27367(17) 0.0440(5) Uani 1 1 d . . . . .
H4A H 0.5768 0.4683 0.2867 0.053 Uiso 1 1 calc R U . . .
H4B H 0.4426 0.5388 0.3462 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5027(2) 0.3223(2) -0.21621(15) 0.0430(5) Uani 1 1 d . . . . .
H5A H 0.4504 0.2477 -0.2683 0.052 Uiso 1 1 calc R U . . .
H5B H 0.6007 0.2773 -0.1946 0.052 Uiso 1 1 calc R U . . .
Pd2 Pd 0.0000 0.5000 0.0000 0.02629(9) Uani 1 2 d S . P . .
N3 N 0.2167(2) 0.7952(2) 0.00124(14) 0.0551(5) Uani 1 1 d . . . . .
N4 N -0.10158(19) 0.6085(2) 0.23003(13) 0.0420(4) Uani 1 1 d . . . . .
C6 C 0.1380(2) 0.6877(2) 0.00010(14) 0.0373(4) Uani 1 1 d . . . . .
C7 C -0.0606(2) 0.5671(2) 0.14771(15) 0.0329(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
N2 Pd1 N2 180.0 . 3_665
N2 Pd1 N1 95.06(6) . 3_665
N2 Pd1 N1 84.94(6) 3_665 3_665
N2 Pd1 N1 84.94(6) . .
N2 Pd1 N1 95.06(6) 3_665 .
N1 Pd1 N1 180.0 3_665 .
C5 N1 C1 112.75(14) . .
C5 N1 Pd1 116.31(12) . .
C1 N1 Pd1 107.12(11) . .
C5 N1 H1 106.7 . .
C1 N1 H1 106.7 . .
Pd1 N1 H1 106.7 . .
C2 N2 C3 112.71(14) . .
C2 N2 Pd1 107.38(10) . .
C3 N2 Pd1 115.02(11) . .
C2 N2 H2 107.1 . .
C3 N2 H2 107.1 . .
Pd1 N2 H2 107.1 . .
N1 C1 C2 108.06(14) . .
N1 C1 H1A 110.1 . .
C2 C1 H1A 110.1 . .
N1 C1 H1B 110.1 . .
C2 C1 H1B 110.1 . .
H1A C1 H1B 108.4 . .
N2 C2 C1 108.17(15) . .
N2 C2 H2A 110.1 . .
C1 C2 H2A 110.1 . .
N2 C2 H2B 110.1 . .
C1 C2 H2B 110.1 . .
H2A C2 H2B 108.4 . .
N2 C3 C4 111.89(16) . .
N2 C3 H3A 109.2 . .
C4 C3 H3A 109.2 . .
N2 C3 H3B 109.2 . .
C4 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
C3 C4 C5 115.09(17) . 3_665
C3 C4 H4A 108.5 . .
C5 C4 H4A 108.5 3_665 .
C3 C4 H4B 108.5 . .
C5 C4 H4B 108.5 3_665 .
H4A C4 H4B 107.5 . .
N1 C5 C4 112.36(16) . 3_665
N1 C5 H5A 109.1 . .
C4 C5 H5A 109.1 3_665 .
N1 C5 H5B 109.1 . .
C4 C5 H5B 109.1 3_665 .
H5A C5 H5B 107.9 . .
C7 Pd2 C7 180.0 . 3_565
C7 Pd2 C6 90.02(7) . 3_565
C7 Pd2 C6 89.98(7) 3_565 3_565
C7 Pd2 C6 89.98(7) . .
C7 Pd2 C6 90.02(7) 3_565 .
C6 Pd2 C6 180.0 3_565 .
N3 C6 Pd2 179.32(17) . .
N4 C7 Pd2 176.71(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N2 2.0447(14) .
Pd1 N2 2.0447(14) 3_665
Pd1 N1 2.0459(14) 3_665
Pd1 N1 2.0459(14) .
N1 C5 1.481(2) .
N1 C1 1.491(2) .
N1 H1 0.9900 .
N2 C2 1.485(2) .
N2 C3 1.488(2) .
N2 H2 0.9900 .
C1 C2 1.509(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C3 C4 1.513(3) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C4 C5 1.516(3) 3_665
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 C4 1.516(3) 3_665
C5 H5A 0.9800 .
C5 H5B 0.9800 .
Pd2 C7 1.9955(19) .
Pd2 C7 1.9955(19) 3_565
Pd2 C6 2.007(2) 3_565
Pd2 C6 2.007(2) .
N3 C6 1.147(3) .
N4 C7 1.146(2) .
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
C5 N1 C1 C2 170.13(15) . . . .
Pd1 N1 C1 C2 40.92(17) . . . .
C3 N2 C2 C1 168.36(14) . . . .
Pd1 N2 C2 C1 40.67(16) . . . .
N1 C1 C2 N2 -55.03(19) . . . .
C2 N2 C3 C4 178.69(15) . . . .
Pd1 N2 C3 C4 -57.76(18) . . . .
N2 C3 C4 C5 71.9(2) . . . 3_665
C1 N1 C5 C4 -178.92(16) . . . 3_665
Pd1 N1 C5 C4 -54.62(19) . . . 3_665
