Synthesis and crystal structure of poly[[di-μ~3~-tetrathioantimonato-tris[(cyclam)cobalt(II)]] acetonitrile disolvate dihydrate] (cyclam = 1,4,8,11-tetraazacyclotetradecane)
Näther, Christian; Danker, Felix; Bensch, Wolfgang; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022001074

data_2244035
_publ_section_title
;
 Synthesis and crystal structure of
 poly[[di-\m~3~-tetrathioantimonato-tris[(cyclam)cobalt(II)]] acetonitrile
 disolvate dihydrate] (cyclam = 1,4,8,11-tetraazacyclotetradecane)
;
_journal_coeditor_code           MW2184
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022001074
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Co3 (Sb S4)2 (C10 H24 N4)3], 2C2 H3 N, 2H2 O'
_chemical_formula_moiety         (SbS4)2,(CoC10H24N4)3,(H2O)2,(CH3CN)2
_chemical_formula_sum            'C34 H82 Co3 N14 O2 S8 Sb2'
_chemical_formula_weight         1395.90
_chemical_name_systematic
;
Poly[[di-\m~3~-tetrathioantimonato-tris[(cyclam)cobalt(II)]]
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-2016/6
_cell_angle_alpha                66.218(3)
_cell_angle_beta                 77.035(3)
_cell_angle_gamma                83.321(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7292(3)
_cell_length_b                   12.9680(5)
_cell_length_c                   13.8936(5)
_cell_measurement_reflns_used    15304
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.003
_cell_measurement_theta_min      1.633
_cell_volume                     1401.93(10)
_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
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15304
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.003
_diffrn_reflns_theta_min         1.633
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  0.7735
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red and X-Shape; Stoe, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             711
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.808
_refine_diff_density_min         -1.564
_refine_ls_extinction_coef       0.0136(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2016/6</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6098
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.1597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                5078
_reflns_number_total             6098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2184sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1401.93(9)
_cod_database_code               2244035
_shelx_hkl_checksum              89746
_shelx_res_checksum              24569
_cod_database_fobs_code 2244035