#------------------------------------------------------------------------------
#$Date: 2022-11-08 12:08:51 +0200 (Tue, 08 Nov 2022) $
#$Revision: 279092 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/60/8106013.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_8106013
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Crystal structure of (1,4,8,11-tetraazacyclotetradecane)palladium(II)
 tetracyanoplatinate(II), C14H24N8PdPt
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1297
_journal_page_last               1298
_journal_paper_doi               10.1515/ncrs-2019-0421
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C10 H24 N4 Pd, C4 N4 Pt'
_chemical_formula_sum            'C14 H24 N8 Pd Pt'
_chemical_formula_weight         605.90
_chemical_name_systematic
;
(1,4,8,11-Tetraazacyclotetradecane)palladium(II) tetracyanoplatinate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 123.8260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0747(3)
_cell_length_b                   8.3376(3)
_cell_length_c                   14.4578(6)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.70
_cell_volume                     908.73(6)
_computing_cell_refinement       'Bruker SAINT [1]'
_computing_data_collection       'Bruker APEX2 [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'ORTEP-III [3]'
_computing_publication_material  'SHELXL-2014/7 [2]'
_computing_structure_refinement  'SHELXL-2014/7 [2]'
_computing_structure_solution    'SHELXL-2014/7 [2]'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27411
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_min         2.702
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.692
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016) [1]'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_description       Block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00102(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0115
_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)+(0.0019P)²+0.5475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0212
_refine_ls_wR_factor_ref         0.0235
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1402
_reflns_number_total             1802
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0421_suppl.cif
_cod_data_source_block           Pd(cyclam)Pt(CN)4
_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_sg_symbol_H-M      'P 21/c'
_cod_database_code               8106013
_shelx_shelxl_version_number     2014/7
_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   0.376
_shelx_estimated_absorpt_t_max   0.581
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5000 0.01966(5) Uani 1 2 d S . P . .
N1 N 0.6713(3) 0.3347(2) 0.61287(16) 0.0255(4) Uani 1 1 d . . . . .
H1 H 0.613(3) 0.286(3) 0.635(2) 0.033(7) Uiso 1 1 d . . . . .
N2 N 0.4614(3) 0.3363(2) 0.38349(16) 0.0274(4) Uani 1 1 d . . . . .
H2 H 0.521(3) 0.369(3) 0.3619(19) 0.027(7) Uiso 1 1 d . . . . .
C1 C 0.7069(3) 0.2148(3) 0.5517(2) 0.0332(6) Uani 1 1 d . . . . .
H1A H 0.7535 0.1158 0.5952 0.040 Uiso 1 1 calc R U . . .
H1B H 0.7952 0.2567 0.5390 0.040 Uiso 1 1 calc R U . . .
C2 C 0.5351(3) 0.1811(3) 0.4418(2) 0.0334(6) Uani 1 1 d . . . . .
H2A H 0.5565 0.1099 0.3965 0.040 Uiso 1 1 calc R U . . .
H2B H 0.4511 0.1286 0.4543 0.040 Uiso 1 1 calc R U . . .
C3 C 0.2788(3) 0.3213(3) 0.28359(19) 0.0364(6) Uani 1 1 d . . . . .
H3A H 0.2023 0.2769 0.3053 0.044 Uiso 1 1 calc R U . . .
H3B H 0.2785 0.2460 0.2314 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2036(3) 0.4807(3) 0.22556(19) 0.0370(6) Uani 1 1 d . . . . .
H4A H 0.0935 0.4604 0.1530 0.044 Uiso 1 1 calc R U . . .
H4B H 0.2879 0.5300 0.2120 0.044 Uiso 1 1 calc R U . . .
C5 C 0.1646(3) 0.5991(3) 0.2888(2) 0.0339(6) Uani 1 1 d . . . . .
H5A H 0.0927 0.6872 0.2391 0.041 Uiso 1 1 calc R U . . .
H5B H 0.0955 0.5455 0.3131 0.041 Uiso 1 1 calc R U . . .
Pt1 Pt 0.0000 0.0000 0.0000 0.02245(5) Uani 1 2 d S . P . .
N3 N 0.3336(3) -0.1092(2) 0.22936(17) 0.0350(5) Uani 1 1 d . . . . .
N4 N 0.2139(3) 0.2958(3) -0.00079(19) 0.0480(6) Uani 1 1 d . . . . .
C6 C 0.2092(3) -0.0686(3) 0.14660(19) 0.0259(5) Uani 1 1 d . . . . .
C7 C 0.1366(3) 0.1879(3) 0.00002(19) 0.0301(5) 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'
Pt Pt -1.7033 8.3905 '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
N1 Pd1 N1 180.0 3_666 .
N1 Pd1 N2 95.00(8) 3_666 .
N1 Pd1 N2 85.00(8) . .
N1 Pd1 N2 85.00(8) 3_666 3_666
N1 Pd1 N2 95.00(8) . 3_666
N2 Pd1 N2 180.0 . 3_666
C5 N1 C1 112.75(18) 3_666 .
C5 N1 Pd1 115.38(15) 3_666 .
C1 N1 Pd1 107.46(14) . .
C5 N1 H1 108.4(16) 3_666 .
C1 N1 H1 107.0(16) . .
Pd1 N1 H1 105.3(17) . .
C3 N2 C2 112.75(19) . .
C3 N2 Pd1 116.59(15) . .
C2 N2 Pd1 107.33(14) . .
C3 N2 H2 106.3(17) . .
C2 N2 H2 108.7(17) . .
Pd1 N2 H2 104.6(17) . .
N1 C1 C2 108.21(19) . .
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 108.10(19) . .
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 112.4(2) . .
N2 C3 H3A 109.1 . .
C4 C3 H3A 109.1 . .
N2 C3 H3B 109.1 . .
C4 C3 H3B 109.1 . .
H3A C3 H3B 107.9 . .
C3 C4 C5 114.9(2) . .
C3 C4 H4A 108.5 . .
C5 C4 H4A 108.5 . .
C3 C4 H4B 108.5 . .
C5 C4 H4B 108.5 . .
H4A C4 H4B 107.5 . .
N1 C5 C4 112.00(19) 3_666 .
N1 C5 H5A 109.2 3_666 .
C4 C5 H5A 109.2 . .
N1 C5 H5B 109.2 3_666 .
C4 C5 H5B 109.2 . .
H5A C5 H5B 107.9 . .
C6 Pt1 C6 180.0 . 3
C6 Pt1 C7 89.94(9) . 3
C6 Pt1 C7 90.06(9) 3 3
C6 Pt1 C7 90.06(9) . .
C6 Pt1 C7 89.94(9) 3 .
C7 Pt1 C7 180.00(16) 3 .
N3 C6 Pt1 177.3(2) . .
N4 C7 Pt1 179.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.0381(19) 3_666
Pd1 N1 2.0381(18) .
Pd1 N2 2.0408(19) .
Pd1 N2 2.0408(19) 3_666
N1 C5 1.478(3) 3_666
N1 C1 1.485(3) .
N1 H1 0.86(2) .
N2 C3 1.478(3) .
N2 C2 1.485(3) .
N2 H2 0.81(2) .
C1 C2 1.508(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C3 C4 1.516(3) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C4 C5 1.516(3) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 N1 1.478(3) 3_666
C5 H5A 0.9800 .
C5 H5B 0.9800 .
Pt1 C6 1.986(2) .
Pt1 C6 1.986(2) 3
Pt1 C7 1.998(2) 3
Pt1 C7 1.998(2) .
N3 C6 1.148(3) .
N4 C7 1.145(3) .
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 -168.52(19) 3_666 . . .
Pd1 N1 C1 C2 -40.3(2) . . . .
C3 N2 C2 C1 -170.4(2) . . . .
Pd1 N2 C2 C1 -40.7(2) . . . .
N1 C1 C2 N2 54.5(2) . . . .
C2 N2 C3 C4 179.16(19) . . . .
Pd1 N2 C3 C4 54.3(2) . . . .
N2 C3 C4 C5 -69.4(3) . . . .
C3 C4 C5 N1 71.6(3) . . . 3_666
