Synthesis, crystal structure and properties of μ-tetrathioantimonato-bis[(cyclam)zinc(II)] perchlorate 0.8-hydrate
Näther, Christian; Lühmann, Henning; Bensch, Wolfgang; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1151–1156; doi:10.1107/S2056989024009356

data_2023275
_publ_section_title
;
 Synthesis, crystal structure and properties of
 \m-tetrathioantimonato-bis[(cyclam)zinc(II)] perchlorate 0.8-hydrate
;
_journal_coeditor_code           HB8108
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1151
_journal_page_last               1156
_journal_paper_doi               10.1107/S2056989024009356
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Zn2 (Sb S4) (C10 H24 N4)2] Cl O4, 0.8H2 O'
_chemical_formula_moiety         'C20 H48 N8 S4 Sb Zn2 +, Cl O4 -, 0.8(H2 O)'
_chemical_formula_sum            'C20 H49.6 Cl N8 O4.8 S4 Sb Zn2'
_chemical_formula_weight         895.25
_chemical_name_systematic
'(\m-Tetrathioantimonato-\k^2^<i>S</i>:<i>S</i>')bis[(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)zinc(II)] perchlorate 0.8-hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9206(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.11238(7)
_cell_length_b                   13.67434(10)
_cell_length_c                   27.49214(18)
_cell_measurement_reflns_used    77740
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.8260
_cell_measurement_theta_min      2.6680
_cell_volume                     3421.23(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            112309
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.793
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.160
_refine_diff_density_min         -0.584
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.408(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         24308
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.8205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                23520
_reflns_number_total             24308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8108.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023275.cif.'
_cod_original_formula_sum        'C20 H49.60 Cl N8 O4.80 S4 Sb Zn2'
_cod_database_code               2023275
_shelx_estimated_absorpt_t_min   0.631
_shelx_estimated_absorpt_t_max   0.702
_shelx_hkl_checksum              21681
_shelx_res_checksum              69131