Crystal structure of catena-poly[(1,4,8,11-tetraazacyclotetradecane-κ 4 N,N′,N″,N′′′)-bis(μ 2-thiocyanato-κ2 N:S)-bis(thiocyanato-κS)-nickel(II)palladium(II)], C14H24N8NiPdS4
Ha, Kwang; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 631–633; doi:10.1515/ncrs-2021-0025

data_8104786
_publ_section_title
;
 Crystal structure of catena-poly[(1,4,8,11-tetraazacyclotetradecane-\k 4
 N,N&#x2032;,N&#x2033;,N&#x2032;&#x2032;&#x2032;)-bis(\m 2-thiocyanato-\k2
 N:S)-bis(thiocyanato-\kS)-nickel(II)palladium(II)], C14H24N8NiPdS4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              631
_journal_page_last               633
_journal_paper_doi               10.1515/ncrs-2021-0025
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C14 H24 N8 Ni Pd S4'
_chemical_formula_sum            'C14 H24 N8 Ni Pd S4'
_chemical_formula_weight         597.76
_chemical_name_systematic
;
<i>catena</i>-[(1,4,8,11-Tetraazacyclotetradecane-\k^4^<i>N,N',N'',N'''</i>)-
bis(\m~2~-thiocyanato-<i>S,N</i>)-bis(thiocyanato-\k<i>S</i>)-nickel(II)-
palladium(II)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.768(3)
_cell_angle_beta                 71.917(3)
_cell_angle_gamma                87.899(3)
_cell_formula_units_Z            4
_cell_length_a                   12.0330(8)
_cell_length_b                   12.0959(8)
_cell_length_c                   15.9551(12)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.54
_cell_volume                     2201.3(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56699
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.064
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.070
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016) [1]'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+7.6847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7640
_reflns_number_total             8670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0025_suppl.cif
_cod_data_source_block           Ni(cyclam)Pd(SCN)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_database_code               8104786
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.820