#------------------------------------------------------------------------------
#$Date: 2022-04-04 12:41:24 +0300 (Mon, 04 Apr 2022) $
#$Revision: 274324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/50/8105022.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_8105022
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Crystal structure of
 (1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N′′′)palladium(II)
 tetracyanonickelate(II), C14H24N8NiPd
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              77
_journal_page_last               78
_journal_paper_doi               10.1515/ncrs-2019-0497
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C10 H24 N4 Pd, C4 N4 Ni'
_chemical_formula_sum            'C14 H24 N8 Ni Pd'
_chemical_formula_weight         469.52
_chemical_name_systematic
;
(1,4,8,11-Tetraazacyclotetradecane)palladium(II) tetracyanonickelate(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                 94.772(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9786(9)
_cell_length_b                   8.3191(9)
_cell_length_c                   11.9489(12)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.96
_cell_volume                     889.42(16)
_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 0.990
_diffrn_measured_fraction_theta_max 0.986
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0082
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22001
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.114
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.083
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016) [1]'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       Block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0161
_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)+(0.0125P)²+0.6811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1560
_reflns_number_total             1744
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0497_suppl.cif
_cod_data_source_block           '[Pd(cyclam)][Ni(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/n'
_cod_database_code               8105022
_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   0.732
_shelx_estimated_absorpt_t_max   0.921
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 0.02139(7) Uani 1 2 d S . P . .
N1 N 0.41795(16) 0.33776(18) -0.11727(12) 0.0284(3) Uani 1 1 d . . . . .
H1 H 0.3156 0.3733 -0.1432 0.034 Uiso 1 1 calc R U . . .
N2 N 0.44102(16) 0.33423(17) 0.11395(11) 0.0269(3) Uani 1 1 d . . . . .
H2 H 0.5332 0.2763 0.1414 0.032 Uiso 1 1 calc R U . . .
C1 C 0.4030(2) 0.1818(2) -0.05848(16) 0.0359(4) Uani 1 1 d . . . . .
H1A H 0.5006 0.1291 -0.0464 0.043 Uiso 1 1 calc R U . . .
H1B H 0.3353 0.1103 -0.1038 0.043 Uiso 1 1 calc R U . . .
C2 C 0.3413(2) 0.2158(2) 0.05258(16) 0.0351(4) Uani 1 1 d . . . . .
H2A H 0.2399 0.2593 0.0404 0.042 Uiso 1 1 calc R U . . .
H2B H 0.3374 0.1165 0.0963 0.042 Uiso 1 1 calc R U . . .
C3 C 0.3755(2) 0.4014(2) 0.21371(15) 0.0348(4) Uani 1 1 d . . . . .
H3A H 0.3525 0.3134 0.2640 0.042 Uiso 1 1 calc R U . . .
H3B H 0.2817 0.4564 0.1898 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4807(2) 0.5185(2) 0.27674(16) 0.0384(5) Uani 1 1 d . . . . .
H4A H 0.5793 0.4679 0.2891 0.046 Uiso 1 1 calc R U . . .
H4B H 0.4444 0.5386 0.3506 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5015(2) 0.3217(2) -0.21876(15) 0.0382(4) Uani 1 1 d . . . . .
H5A H 0.4484 0.2468 -0.2714 0.046 Uiso 1 1 calc R U . . .
H5B H 0.6005 0.2765 -0.1972 0.046 Uiso 1 1 calc R U . . .
Ni1 Ni 0.0000 0.5000 0.0000 0.02491(8) Uani 1 2 d S . P . .
N3 N 0.2140(2) 0.7799(3) 0.00057(15) 0.0485(5) Uani 1 1 d . . . . .
N4 N -0.09581(18) 0.6054(2) 0.22392(13) 0.0368(4) Uani 1 1 d . . . . .
C6 C 0.1330(2) 0.6736(2) -0.00001(14) 0.0325(4) Uani 1 1 d . . . . .
C7 C -0.05582(19) 0.5641(2) 0.14010(15) 0.0284(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'
Ni Ni 0.3393 1.1124 '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 95.04(6) 3_665 .
N2 Pd1 N1 84.96(6) . .
N2 Pd1 N1 84.96(6) 3_665 3_665
N2 Pd1 N1 95.04(6) . 3_665
N1 Pd1 N1 180.0 . 3_665
C5 N1 C1 112.28(14) . .
C5 N1 Pd1 116.29(12) . .
C1 N1 Pd1 107.15(10) . .
C5 N1 H1 106.9 . .
C1 N1 H1 106.9 . .
Pd1 N1 H1 106.9 . .
C3 N2 C2 112.62(14) . .
C3 N2 Pd1 115.14(11) . .
C2 N2 Pd1 107.38(10) . .
C3 N2 H2 107.1 . .
C2 N2 H2 107.1 . .
Pd1 N2 H2 107.1 . .
N1 C1 C2 107.83(15) . .
N1 C1 H1A 110.1 . .
C2 C1 H1A 110.1 . .
N1 C1 H1B 110.1 . .
C2 C1 H1B 110.1 . .
H1A C1 H1B 108.5 . .
N2 C2 C1 108.04(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 111.72(15) . .
N2 C3 H3A 109.3 . .
C4 C3 H3A 109.3 . .
N2 C3 H3B 109.3 . .
C4 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
C3 C4 C5 115.03(16) . 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 112.00(16) . 3_665
N1 C5 H5A 109.2 . .
C4 C5 H5A 109.2 3_665 .
N1 C5 H5B 109.2 . .
C4 C5 H5B 109.2 3_665 .
H5A C5 H5B 107.9 . .
C7 Ni1 C7 180.0 3_565 .
C7 Ni1 C6 89.91(8) 3_565 3_565
C7 Ni1 C6 90.09(8) . 3_565
C7 Ni1 C6 90.09(8) 3_565 .
C7 Ni1 C6 89.91(8) . .
C6 Ni1 C6 180.0 3_565 .
N3 C6 Ni1 179.62(18) . .
N4 C7 Ni1 177.10(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N2 2.0386(14) 3_665
Pd1 N2 2.0386(14) .
Pd1 N1 2.0386(14) .
Pd1 N1 2.0386(14) 3_665
N1 C5 1.484(2) .
N1 C1 1.487(2) .
N1 H1 0.9900 .
N2 C3 1.482(2) .
N2 C2 1.483(2) .
N2 H2 0.9900 .
C1 C2 1.507(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 1.514(3) 3_665
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 C4 1.514(3) 3_665
C5 H5A 0.9800 .
C5 H5B 0.9800 .
Ni1 C7 1.8648(18) 3_565
Ni1 C7 1.8649(18) .
Ni1 C6 1.874(2) 3_565
Ni1 C6 1.874(2) .
N3 C6 1.145(3) .
N4 C7 1.144(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 170.29(15) . . . .
Pd1 N1 C1 C2 41.43(16) . . . .
C3 N2 C2 C1 168.44(15) . . . .
Pd1 N2 C2 C1 40.66(16) . . . .
N1 C1 C2 N2 -55.29(19) . . . .
C2 N2 C3 C4 178.49(15) . . . .
Pd1 N2 C3 C4 -57.95(17) . . . .
N2 C3 C4 C5 72.2(2) . . . 3_665
C1 N1 C5 C4 -178.72(16) . . . 3_665
Pd1 N1 C5 C4 -54.82(19) . . . 3_665
