1,4,8,11-Tetraazacyclotetradecane antimony(III) sulfide
Lees, Rachel J. E.; Powell, Anthony V.; Watkin, David J.; Chippindale, Ann M.; Acta Crystallographica Section C 63 (2007) m27–m29; doi:10.1107/S010827010605044X

data_2015734
_publ_section_title
;
 1,4,8,11-Tetraazacyclotetradecane antimony(III) sulfide
;
_journal_coeditor_code           GA3032
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m27
_journal_page_last               m29
_journal_paper_doi               10.1107/S010827010605044X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C10 H20 N4) [Sb6 S10]'
_chemical_formula_moiety         'C10 H20 N4 2+, S10 Sb6 2-'
_chemical_formula_sum            'C10 H20 N4 S10 Sb6'
_chemical_formula_weight         1247.46
_chemical_name_systematic
;
Poly[1,4,8,11-tetraazacyclotetradecane(2+)
[hepta-\m-sulfido-trisulfidohexaantimony(III)]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 105.878(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4872(9)
_cell_length_b                   15.4477(14)
_cell_length_c                   10.7567(9)
_cell_measurement_reflns_used    4160
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.23
_cell_volume                     1516.3(2)
_computing_cell_refinement       APEX-2
_computing_data_collection       'APEX-2 (Bruker, 2005)'
_computing_data_reduction        APEX-2
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker--Nonius Apex-2 CCD area-detector diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49836
_diffrn_reflns_theta_full        29.957
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         2.232
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.968
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.16
_refine_diff_density_min         -2.81
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0801
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.007263
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Modified Chebychev polynomial, (Watkin, 1994)
with coefficients
1.00, -1.11, 0.479 and -0.402
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0382
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                4008
_reflns_number_total             4612
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            ga3032.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015734
_cod_database_fobs_code          2015734