Crystal structure of μ~3~-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane)
Näther, Christian; Danker, Felix; Bensch, Wolfgang; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022003759

data_2244071
_publ_section_title
;
 Crystal structure of \m~3~-tetrathioantimonato-tris[(cyclam)zinc(II)]
 tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder
 over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane)
;
_journal_coeditor_code           WM5639
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022003759
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Zn3 (Sb S4) (C10 H24 N4)3] (Sb S4), 2C H3 C N, 2H2 O'
_chemical_formula_moiety
'C30 H72 N12 S4 Sb1 Zn3 3+, S4 Sb1 3-, 2(C2 H4 N1), 2(H2 O1)'
_chemical_formula_sum            'C34 H82 N14 O2 S8 Sb2 Zn3'
_chemical_formula_weight         1415.22
_chemical_name_common
;
\m~3~-Tetrathioantimonato-tris[(1,4,8,11-tetraazacyclotetradecane)zinc(II)]
tetrathioantimonate acetonitrile disolvate dihydrate
;
_chemical_name_systematic
;
\m~3~-Tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate
acetonitrile disolvate dihydrate
;
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                67.018(3)
_cell_angle_beta                 77.677(3)
_cell_angle_gamma                84.220(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7856(3)
_cell_length_b                   13.1738(6)
_cell_length_c                   14.0096(6)
_cell_measurement_reflns_used    14357
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.004
_cell_measurement_theta_min      1.608
_cell_volume                     1458.10(11)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14357
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.004
_diffrn_reflns_theta_min         1.608
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.7808
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED and X-SHAPE; Stoe, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.800
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0289
_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/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                5594
_reflns_number_total             6303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5639sup1.cif
_cod_data_source_block           I
_cod_database_code               2244071
_shelx_hkl_checksum              99572
_shelx_res_checksum              20173
_cod_database_fobs_code 2244071