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###           Full Paper (Acta Crystallographica Section C)                ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
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##############################################################################
data_I
_audit_creation_method     CRYSTALS_ver_12.84
_chemical_name_systematic
;
Poly[1,4,8,11-tetraazacyclotetradecane(2+)
[hepta-μ-sulfido-trisulfidohexaantimony(III)]]
;
_chemical_formula_moiety     'C10 H20 N4 2+, S10 Sb6 2-'
_chemical_formula_sum     'C10 H20 N4 S10 Sb6'
_chemical_formula_iupac     '(C10 H20 N4) [Sb6 S10]'
_chemical_formula_weight     1247.46
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x,y,z'
    '-x,-y,-z'
    '-x,y+1/2,-z+1/2'
    'x,-y+1/2,z+1/2'
_cell_length_a     9.4872(9)
_cell_length_b     15.4477(14)
_cell_length_c     10.7567(9)
_cell_angle_alpha     90
_cell_angle_beta     105.878(4)
_cell_angle_gamma     90
_cell_volume     1516.3(2)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     4160
_cell_measurement_theta_min     2.23
_cell_measurement_theta_max     30.52
_cell_measurement_temperature     100
_exptl_crystal_description     'block'
_exptl_crystal_colour     'orange'
_exptl_crystal_size_max     0.16
_exptl_crystal_size_mid     0.12
_exptl_crystal_size_min     0.06
_exptl_crystal_density_diffrn     2.732
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1148
_exptl_absorpt_coefficient_mu     5.968
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.44
_exptl_absorpt_correction_T_max     0.70
_diffrn_ambient_temperature     100
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator     'graphite'
_diffrn_measurement_device_type
                        'Bruker--Nonius Apex-2 CCD area-detector diffractometer'
_diffrn_measurement_method     ω/2θ
_diffrn_reflns_number     49836
_diffrn_reflns_av_R_equivalents     0.083
_diffrn_reflns_theta_min     2.232
_diffrn_reflns_theta_max     30.568
_diffrn_reflns_theta_full     29.957
_diffrn_measured_fraction_theta_max     0.992
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     13
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     22
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     15
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     0.00
_reflns_number_total     4612
_reflns_number_gt     4008
_reflns_threshold_expression     I>3.0σ(I)
_refine_ls_structure_factor_coef     F
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0554
_refine_ls_R_factor_gt     0.0492
_refine_ls_wR_factor_all     0.0382
_refine_ls_wR_factor_gt     0.0377
_refine_ls_wR_factor_ref     0.0377
_refine_ls_goodness_of_fit_ref     1.0801
_refine_ls_number_reflns     4008
_refine_ls_number_parameters     150
_refine_ls_number_restraints     72
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
;
Modified Chebychev polynomial, (Watkin, 1994)
with coefficients
1.00, -1.11, 0.479 and -0.402
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_refine_ls_shift/su_max     0.007263
_refine_diff_density_max     3.16
_refine_diff_density_min     -2.81
_refine_ls_extinction_method     'None'
loop_
    _atom_type_symbol
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
    H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
    N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
    S 0.1246 0.1234 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
    Sb -0.5866 1.5461 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'APEX-2 (Bruker, 2005)'
_computing_cell_refinement     'APEX-2'
_computing_data_reduction     'APEX-2'
_computing_structure_solution     'SIR92 (Altomare et al.,  1994)'
_computing_structure_refinement     'CRYSTALS (Betteridge et al.,  2003)'
_computing_molecular_graphics     'ATOMS (Dowty, 2000)'
_computing_publication_material     'CRYSTALS'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Sb Sb1 1.00384(4) 1.08793(2) 0.65826(4) 0.0091 Uani 1 . .
    Sb Sb2 0.97163(4) 0.62304(2) 0.50401(4) 0.0103 Uani 1 . .
    Sb Sb3 1.01909(4) 0.8336(2) 0.68011(4) 0.0102 Uani 1 . .
    S S1 1.16052(15) 0.63947(9) 0.71266(14) 0.0109 Uani 1 . .
    S S2 0.84366(15) 0.50475(9) 0.56996(15) 0.0115 Uani 1 . .
    S S3 0.81632(17) 0.73823(10) 0.58957(19) 0.0187 Uani 1 . .
    S S4 0.85825(15) 0.95669(9) 0.58297(14) 0.0115 Uani 1 . .
    S S5 1.15565(16) 0.8234(10) 0.51501(15) 0.0134 Uani 1 . .
    N N1 0.4837(6) 1.1163(3) 0.0497(6) 0.0337 Uani 1 . .
    N N2 0.4565(6) 0.9642(4) 0.1723(5) 0.0291 Uani 1 . .
    C C1 0.515(2) 1.1615(8) 0.1700(12) 0.0498 Uani 0.5 1 2
    C C2 0.4566(17) 1.1105(8) 0.2678(11) 0.0515 Uani 0.5 1 2
    C C3 0.5160(2) 1.0191(8) 0.2928(10) 0.0533 Uani 0.5 1 2
    C C4 0.5149(17) 0.8740(6) 0.1742(9) 0.0453 Uani 0.5 1 2
    C C5 0.4599(17) 0.8345(7) 0.0411(10) 0.0496 Uani 0.5 1 2
    C C11 0.542(2) 1.1501(10) 0.1799(11) 0.0498 Uani 0.5 1 1
    C C21 0.4665(16) 1.1067(8) 0.2728(10) 0.0515 Uani 0.5 1 1
    C C31 0.502(2) 1.0129(7) 0.2972(8) 0.0533 Uani 0.5 1 1
    C C41 0.5109(16) 0.8729(6) 0.1723(9) 0.0453 Uani 0.5 1 1
    C C51 0.4557(17) 0.8354(7) 0.0384(9) 0.0496 Uani 0.5 1 1
    H H21 0.4826 1.1417 0.3494 0.0611 Uiso 0.5 1 2
    H H22 0.3506 1.1074 0.2352 0.0611 Uiso 0.5 1 2
    H H31 0.4862 0.9938 0.3643 0.064 Uiso 0.5 1 2
    H H32 0.6223 1.0205 0.3139 0.064 Uiso 0.5 1 2
    H H41 0.482 0.8396 0.2364 0.057 Uiso 0.5 1 2
    H H42 0.6213 0.8757 0.1986 0.057 Uiso 0.5 1 2
    H H51 0.3535 0.8363 0.0142 0.063 Uiso 0.5 1 2
    H H52 0.4932 0.775 0.0433 0.0631 Uiso 0.5 1 2
    H H111 0.525 1.212 0.1791 0.0591 Uiso 0.5 1 1
    H H112 0.6466 1.1387 0.2091 0.059 Uiso 0.5 1 1
    H H211 0.4958 1.137 0.3552 0.0611 Uiso 0.5 1 1
    H H212 0.3613 1.1122 0.2362 0.0611 Uiso 0.5 1 1
    H H311 0.4515 0.9898 0.3569 0.064 Uiso 0.5 1 1
    H H312 0.6073 1.0063 0.334 0.064 Uiso 0.5 1 1
    H H411 0.4759 0.8385 0.2332 0.057 Uiso 0.5 1 1
    H H412 0.6173 0.8731 0.1974 0.057 Uiso 0.5 1 1
    H H511 0.3494 0.8393 0.0105 0.063 Uiso 0.5 1 1
    H H512 0.4857 0.7752 0.0395 0.0632 Uiso 0.5 1 1
    H H11 0.4691 1.2183 0.1564 0.0591 Uiso 0.5 1 2
    H H12 0.6202 1.168 0.2039 0.059 Uiso 0.5 1 2
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Sb1 0.00918(14) 0.00665(14) 0.01075(15) 0.00060(12) 0.00176(12) -0.00020(12)
    Sb2 0.01056(15) 0.00842(14) 0.01083(16) 0.00027(13) 0.00106(12) 0.00012(13)
    Sb3 0.01191(16) 0.00749(14) 0.01076(15) 0.00031(13) 0.00243(12) -0.00037(13)
    S1 0.0103(6) 0.0105(6) 0.0119(6) -0.0018(5) 0.0030(5) -0.0005(5)
    S2 0.0098(6) 0.0080(5) 0.0153(6) -0.0011(5) 0.0009(5) -0.0017(5)
    S3 0.0115(6) 0.0090(6) 0.0368(9) -0.0013(5) 0.0086(6) -0.0052(6)
    S4 0.0120(6) 0.0066(5) 0.0156(6) 0.0001(5) 0.0033(5) -0.0010(5)
    S5 0.0117(6) 0.0128(6) 0.0167(6) 0.0050(5) 0.0054(5) 0.0049(5)
    N1 0.011(2) 0.015(3) 0.075(6) -0.003(2) 0.012(3) -0.011(3)
    N2 0.012(2) 0.045(4) 0.031(3) 0.005(3) 0.007(2) 0.017(3)
    C1 0.038(5) 0.049(4) 0.061(4) 0.003(3) 0.009(5) -0.024(4)
    C2 0.042(4) 0.066(4) 0.043(4) 0.000(3) 0.006(4) -0.034(3)
    C3 0.040(4) 0.078(4) 0.044(4) 0.003(3) 0.013(5) -0.004(4)
    C4 0.032(3) 0.049(4) 0.063(4) 0.012(3) 0.027(4) 0.031(3)
    C5 0.0512(10) 0.0508(10) 0.0540(10) 0.0071(7) 0.026(4) 0.0005(10)
    C11 0.038(5) 0.049(4) 0.061(4) 0.003(3) 0.009(5) -0.024(4)
    C21 0.042(4) 0.066(4) 0.043(4) 0.000(3) 0.006(4) -0.034(3)
    C31 0.040(4) 0.078(4) 0.044(4) 0.003(3) 0.013(5) -0.004(4)
    C41 0.032(3) 0.049(4) 0.063(4) 0.012(3) 0.027(4) 0.031(3)
    C51 0.0512(10) 0.0508(10) 0.0540(10) 0.0071(7) 0.026(4) 0.0005(10)
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Sb1 S1 . 3_756 2.4855(15) yes
    Sb1 S5 . 2_776 2.469(9) yes
    Sb1 S4 . . 2.4621(14) yes
    Sb2 S2 . 2_766 2.8920(15) yes
    Sb2 S1 . . 2.4723(15) yes
    Sb2 S2 . . 2.4059(15) yes
    Sb2 S3 . . 2.6319(16) yes
    Sb3 S3 . . 2.4072(16) yes
    Sb3 S4 . . 2.4826(15) yes
    Sb3 S5 . . 2.4730(15) yes
    N1 C5 . 2_675 1.450(9) no
    N1 C1 . . 1.429(9) no
    N2 C3 . . 1.522(9) no
    N2 C4 . . 1.497(9) no
    C1 C2 . . 1.534(10) no
    C1 H11 . . 0.971 no
    C1 H12 . . 0.972 no
    C2 C3 . . 1.517(9) no
    C2 H21 . . 0.973 no
    C2 H22 . . 0.971 no
    C3 H31 . . 0.972 no
    C3 H32 . . 0.971 no
    C4 C5 . . 1.512(9) no
    C4 H41 . . 0.971 no
    C4 H42 . . 0.971 no
    C5 H51 . . 0.972 no
    C5 H52 . . 0.971 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    S1 Sb1 S5 3_756 . 2_776 84.00(5) yes
    S1 Sb1 S4 3_756 . . 93.80(5) yes
    S5 Sb1 S4 2_776 . . 92.05(5) yes
    S2 Sb2 S1 2_766 . . 88.66(5) yes
    S2 Sb2 S2 2_766 . . 87.44(5) yes
    S1 Sb2 S2 . . . 96.27(5) yes
    S1 Sb2 S3 . . . 87.09(5) yes
    S2 Sb2 S3 . . . 91.97(5) yes
    S3 Sb3 S4 . . . 88.13(5) yes
    S3 Sb3 S5 . . . 100.8(2) yes
    S4 Sb3 S5 . . . 97.4(3) yes
    C5 N1 C1 2_675 . . 109.35(10) no
    C3 N2 C4 . . . 117.22(10) no
    N1 C1 C2 . . . 110.25(10) no
    N1 C1 H11 . . . 109.4 no
    C2 C1 H11 . . . 109.8 no
    N1 C1 H12 . . . 109.0 no
    C2 C1 H12 . . . 108.8 no
    H11 C1 H12 . . . 109.6 no
    C1 C2 C3 . . . 114.44(10) no
    C1 C2 H21 . . . 108.3 no
    C3 C2 H21 . . . 108.2 no
    C1 C2 H22 . . . 108.0 no
    C3 C2 H22 . . . 108.4 no
    H21 C2 H22 . . . 109.4 no
    N2 C3 C2 . . . 109.57(10) no
    N2 C3 H31 . . . 109.3 no
    C2 C3 H31 . . . 109.8 no
    N2 C3 H32 . . . 109.4 no
    C2 C3 H32 . . . 109.5 no
    H31 C3 H32 . . . 109.3 no
    N2 C4 C5 . . . 109.39(10) no
    N2 C4 H41 . . . 109.3 no
    C5 C4 H41 . . . 109.8 no
    N2 C4 H42 . . . 109.4 no
    C5 C4 H42 . . . 109.3 no
    H41 C4 H42 . . . 109.6 no
    C4 C5 N1 . . 2_675 109.35(10) no
    C4 C5 H51 . . . 109.4 no
    N1 C5 H51 2_675 . . 109.2 no
    C4 C5 H52 . . . 109.5 no
    N1 C5 H52 2_675 . . 109.6 no
    H51 C5 H52 . . . 109.9 no
data_global
_journal_date_recd_electronic     2006-10-24
_journal_date_accepted     2006-11-22
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2007
_journal_volume     63
_journal_issue      1
_journal_page_first     m27
_journal_page_last     m29
_journal_paper_category     FM
_journal_coeditor_code     GA3032
_publ_contact_author_name     'A. V. Powell'
_publ_contact_author_address
;
Department of Chemistry,
Heriot-Watt University,
Edinburgh
EH14 4AS, UK
;
_publ_contact_author_email     a.v.powell@hw.ac.uk
_publ_contact_author_fax     '+44 131 4513180'
_publ_contact_author_phone     '+44 131 4518034'
_publ_section_title
;
1,4,8,11-Tetraazacyclotetradecane antimony(III) sulfide
;
loop_
    _publ_author_name
    _publ_author_address
    'Lees, Rachel J. E.'
;
Department of Chemistry
Heriot--Watt University
Edinburgh EH14 4AS
Scotland
;
    'Powell, Anthony V.'
;
Department of Chemistry
Heriot--Watt University
Edinburgh EH14 4AS
Scotland
;
    'Watkin, David J.'
;
Chemical Crystallography Laboratory
Chemistry Research Laboratory
University of Oxford
Oxford OX1 3TA
England
;
    'Chippindale, Ann M.'
;
School of Chemistry
The University of Reading
Whiteknights
Reading RG6 6AD
England
;
_publ_section_synopsis
;
Poly[1,4,8,11-tetraazacyclotetradecane(2+)
[hepta-μ-sulfido-trisulfidohexaantimony(III)]],
{(C₁₀H₂₆N₄)[Sb₆S₁₀]}ₙ, was synthesized solvothermally
using the macrocyclic tetramine 1,4,8,11-tetraazacyclotetradecane (cyclam) as
the structure-directing agent. The structure consists of novel
[Sb₆S₁₀]²⁻ layers containing Sb₂S₂, Sb₄S₄ and Sb₇S₇
hetero-rings, which are separated by macrocyclic amine molecules. The
macrocyle amine molecules are disordered over two crystallographically
distinct positions and diprotonated in order to balance the charge of the
anionic layers.
;
