#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/29/7202936.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7202936
loop_
_publ_author_name
'Benson, Ronald E.'
'Ellis, Carol A.'
'Lewis, Clairissa E.'
'Tiekink, Edward R.T.'
_publ_section_title
;
 3D-, 2D- and 1D-supramolecular structures of {Zn[S2CN(CH2CH2OH)R]2}2
 and their {Zn[S2CN(CH2CH2OH)R]2}2(4,4′-bipyridine) adducts for
 R = CH2CH2OH, Me or Et: polymorphism and pseudo-polymorphism
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              930
_journal_paper_doi               10.1039/b706442j
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C30 H48 N6 O4 S8 Zn2'
_chemical_formula_sum            'C30 H48 N6 O4 S8 Zn2'
_chemical_formula_weight         943.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.546(7)
_cell_angle_beta                 107.095(15)
_cell_angle_gamma                92.740(8)
_cell_formula_units_Z            2
_cell_length_a                   11.074(6)
_cell_length_b                   13.249(5)
_cell_length_c                   15.350(6)
_cell_measurement_reflns_used    1442
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      3.1
_cell_volume                     2065.6(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  AFC12Κ/SATURN724
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43962
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.8
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.47
_refine_diff_density_min         -0.96
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.10
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.10
_refine_ls_R_factor_all          0.064
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0882P)²+2.5657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.162
_refine_ls_wR_factor_ref         0.168
_reflns_number_gt                8729
_reflns_number_total             9411
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b706442j.txt
_cod_data_source_block           (5)
_cod_original_cell_volume        2065.5(15)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               7202936
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.40370(4) 0.72052(3) 0.55437(3) 0.03438(13) Uani 1 1 d . . .
Zn2 Zn 0.63665(4) 0.24286(3) -0.07473(3) 0.03441(13) Uani 1 1 d . . .
S1 S 0.48523(8) 0.89867(7) 0.59924(6) 0.0350(2) Uani 1 1 d . . .
S2 S 0.63266(8) 0.73931(7) 0.66754(7) 0.0360(2) Uani 1 1 d . . .
S3 S 0.28323(8) 0.61902(7) 0.61367(7) 0.0367(2) Uani 1 1 d . . .
S4 S 0.16429(8) 0.73715(7) 0.47954(6) 0.0351(2) Uani 1 1 d . . .
S5 S 0.54742(9) 0.06668(7) -0.09639(7) 0.0403(2) Uani 1 1 d . . .
S6 S 0.43465(11) 0.20619(8) -0.20986(7) 0.0479(3) Uani 1 1 d . . .
S7 S 0.75485(9) 0.35179(8) -0.13263(7) 0.0419(2) Uani 1 1 d . . .
S8 S 0.87067(9) 0.24275(8) 0.00968(7) 0.0419(2) Uani 1 1 d . . .
O1 O 0.8412(3) 1.04160(10) 0.6122(2) 0.0616(8) Uani 1 1 d D . .
H1O H 0.8278 0.9775 0.5822 0.092 Uiso 1 1 d D . .
O2 O -0.1790 0.8350 0.4998 0.0618(8) Uani 1 1 d D . .
H2O H -0.1566 0.8563 0.4590 0.093 Uiso 1 1 d D . .
O3 O 0.07225(15) 0.1249(3) -0.3692(3) 0.0781(12) Uani 1 1 d D . .
H3O H -0.0025 0.0951 -0.3839 0.117 Uiso 1 1 d D . .
O4 O 1.1122(5) 0.3372(2) -0.2324(3) 0.1176(18) Uani 1 1 d D . .
H4O H 1.0899 0.2783 -0.2732 0.176 Uiso 1 1 d D . .
N1 N 0.7219(3) 0.9442(2) 0.7200(2) 0.0326(6) Uani 1 1 d . . .
N2 N 0.0343(3) 0.6391(2) 0.5629(2) 0.0351(6) Uani 1 1 d . . .
N3 N 0.3323(3) 0.0092(3) -0.2414(2) 0.0446(8) Uani 1 1 d . . .
N4 N 1.0048(3) 0.3580(3) -0.0590(2) 0.0401(7) Uani 1 1 d . . .
N5 N 0.4365(3) 0.6388(2) 0.4317(2) 0.0336(6) Uani 1 1 d . . .
N6 N 0.5854(3) 0.3362(2) 0.0363(2) 0.0340(6) Uani 1 1 d . . .
C1 C 0.6253(3) 0.8690(3) 0.6689(2) 0.0295(6) Uani 1 1 d . . .
C2 C 0.7145(4) 1.0551(3) 0.7198(3) 0.0371(7) Uani 1 1 d . . .
H2A H 0.7809 1.1006 0.7766 0.045 Uiso 1 1 calc R . .
H2B H 0.6305 1.0734 0.7244 0.045 Uiso 1 1 calc R . .
C3 C 0.7321(4) 1.0775(3) 0.6321(3) 0.0479(9) Uani 1 1 d . . .
H3A H 0.6560 1.0436 0.5770 0.058 Uiso 1 1 calc R . .
H3B H 0.7378 1.1543 0.6404 0.058 Uiso 1 1 calc R . .
C4 C 0.8407(3) 0.9219(3) 0.7830(3) 0.0398(8) Uani 1 1 d . . .
H4A H 0.9137 0.9690 0.7841 0.048 Uiso 1 1 calc R . .
H4B H 0.8541 0.8485 0.7574 0.048 Uiso 1 1 calc R . .
C5 C 0.8367(5) 0.9377(4) 0.8836(3) 0.0570(11) Uani 1 1 d . . .
H5A H 0.9168 0.9222 0.9230 0.085 Uiso 1 1 calc R . .
H5B H 0.7654 0.8903 0.8829 0.085 Uiso 1 1 calc R . .
H5C H 0.8252 1.0107 0.9097 0.085 Uiso 1 1 calc R . .
C6 C 0.1482(3) 0.6627(3) 0.5530(2) 0.0301(6) Uani 1 1 d . . .
C7 C -0.0801(3) 0.6776(3) 0.5107(3) 0.0414(8) Uani 1 1 d . . .
H7A H -0.1569 0.6315 0.5045 0.050 Uiso 1 1 calc R . .
H7B H -0.0774 0.6736 0.4461 0.050 Uiso 1 1 calc R . .
C8 C -0.0902(4) 0.7897(4) 0.5598(3) 0.0514(10) Uani 1 1 d . . .
H8A H -0.1159 0.7907 0.6165 0.062 Uiso 1 1 calc R . .
H8B H -0.0055 0.8323 0.5814 0.062 Uiso 1 1 calc R . .
C9 C 0.0191(4) 0.5771(3) 0.6269(3) 0.0418(8) Uani 1 1 d . . .
H9A H 0.0933 0.5381 0.6407 0.050 Uiso 1 1 calc R . .
H9B H -0.0581 0.5248 0.5941 0.050 Uiso 1 1 calc R . .
C10 C 0.0079(8) 0.6424(4) 0.7193(4) 0.096(2) Uani 1 1 d . . .
H10A H -0.0022 0.5963 0.7584 0.144 Uiso 1 1 calc R . .
H10B H -0.0664 0.6802 0.7065 0.144 Uiso 1 1 calc R . .
H10C H 0.0851 0.6931 0.7533 0.144 Uiso 1 1 calc R . .
C11 C 0.4258(4) 0.0867(3) -0.1877(2) 0.0368(7) Uani 1 1 d . . .
C12 C 0.2405(4) 0.0230(3) -0.3261(3) 0.0500(10) Uani 1 1 d . . .
H12A H 0.2826 0.0661 -0.3557 0.060 Uiso 1 1 calc R . .
H12B H 0.2044 -0.0461 -0.3727 0.060 Uiso 1 1 calc R . .
C13 C 0.1395(5) 0.0757(4) -0.2980(4) 0.0607(12) Uani 1 1 d . . .
H13A H 0.0791 0.0238 -0.2901 0.073 Uiso 1 1 calc R . .
H13B H 0.1769 0.1297 -0.2363 0.073 Uiso 1 1 calc R . .
C14 C 0.3214(4) -0.0927(3) -0.2215(3) 0.0492(10) Uani 1 1 d . . .
H14A H 0.4078 -0.1108 -0.1950 0.059 Uiso 1 1 calc R . .
H14B H 0.2776 -0.1476 -0.2815 0.059 Uiso 1 1 calc R . .
C15 C 0.2480(5) -0.0921(4) -0.1518(4) 0.0580(11) Uani 1 1 d . . .
H15A H 0.2424 -0.1617 -0.1408 0.087 Uiso 1 1 calc R . .
H15B H 0.1620 -0.0752 -0.1781 0.087 Uiso 1 1 calc R . .
H15C H 0.2924 -0.0392 -0.0917 0.087 Uiso 1 1 calc R . .
C16 C 0.8909(3) 0.3213(3) -0.0598(2) 0.0348(7) Uani 1 1 d . . .
C17 C 1.0190(4) 0.4233(3) -0.1209(3) 0.0480(9) Uani 1 1 d . . .
H17A H 1.1047 0.4648 -0.0933 0.058 Uiso 1 1 calc R . .
H17B H 0.9556 0.4736 -0.1215 0.058 Uiso 1 1 calc R . .
C18 C 1.0025(6) 0.3630(5) -0.2208(3) 0.0670(14) Uani 1 1 d . . .
H18A H 0.9420 0.2982 -0.2384 0.080 Uiso 1 1 calc R . .
H18B H 0.9654 0.4060 -0.2638 0.080 Uiso 1 1 calc R . .
C19 C 1.1222(4) 0.3332(4) 0.0030(3) 0.0553(11) Uani 1 1 d . . .
H19A H 1.1049 0.3204 0.0594 0.066 Uiso 1 1 calc R . .
H19B H 1.1887 0.3948 0.0255 0.066 Uiso 1 1 calc R . .
C20 C 1.1721(6) 0.2385(6) -0.0455(4) 0.0843(18) Uani 1 1 d . . .
H20A H 1.2494 0.2257 -0.0008 0.126 Uiso 1 1 calc R . .
H20B H 1.1919 0.2515 -0.1002 0.126 Uiso 1 1 calc R . .
H20C H 1.1073 0.1769 -0.0670 0.126 Uiso 1 1 calc R . .
C21 C 0.5420(3) 0.6667(3) 0.4130(2) 0.0356(7) Uani 1 1 d . . .
H21 H 0.5983 0.7270 0.4552 0.043 Uiso 1 1 calc R . .
C22 C 0.5722(3) 0.6112(3) 0.3346(2) 0.0348(7) Uani 1 1 d . . .
H22 H 0.6482 0.6331 0.3239 0.042 Uiso 1 1 calc R . .
C23 C 0.4904(3) 0.5231(2) 0.2717(2) 0.0305(7) Uani 1 1 d . . .
C24 C 0.3793(3) 0.4964(3) 0.2907(2) 0.0339(7) Uani 1 1 d . . .
H24 H 0.3195 0.4381 0.2485 0.041 Uiso 1 1 calc R . .
C25 C 0.3567(3) 0.5549(3) 0.3706(3) 0.0359(7) Uani 1 1 d . . .
H25 H 0.2812 0.5349 0.3830 0.043 Uiso 1 1 calc R . .
C26 C 0.5218(3) 0.4592(3) 0.1890(2) 0.0312(7) Uani 1 1 d . . .
C27 C 0.5926(4) 0.5036(3) 0.1436(3) 0.0401(8) Uani 1 1 d . . .
H27 H 0.6211 0.5770 0.1642 0.048 Uiso 1 1 calc R . .
C28 C 0.6211(4) 0.4394(3) 0.0681(3) 0.0403(8) Uani 1 1 d . . .
H28 H 0.6688 0.4709 0.0372 0.048 Uiso 1 1 calc R . .
C29 C 0.5168(4) 0.2929(3) 0.0797(3) 0.0394(8) Uani 1 1 d . . .
H29 H 0.4902 0.2192 0.0576 0.047 Uiso 1 1 calc R . .
C30 C 0.4833(4) 0.3508(3) 0.1548(3) 0.0386(8) Uani 1 1 d . . .
H30 H 0.4341 0.3173 0.1834 0.046 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Zn1 S1 111.72(9) . . ?
N5 Zn1 S3 114.38(9) . . ?
S1 Zn1 S3 133.77(4) . . ?
N5 Zn1 S2 97.39(9) . . ?
S1 Zn1 S2 73.34(3) . . ?
S3 Zn1 S2 103.54(4) . . ?
N5 Zn1 S4 97.83(9) . . ?
S1 Zn1 S4 98.40(4) . . ?
S3 Zn1 S4 72.41(4) . . ?
S2 Zn1 S4 164.54(3) . . ?
N6 Zn2 S7 109.42(9) . . ?
N6 Zn2 S5 105.78(9) . . ?
S7 Zn2 S5 144.78(4) . . ?
N6 Zn2 S6 102.48(9) . . ?
S7 Zn2 S6 97.17(5) . . ?
S5 Zn2 S6 73.60(4) . . ?
N6 Zn2 S8 99.84(9) . . ?
S7 Zn2 S8 73.06(4) . . ?
S5 Zn2 S8 102.47(4) . . ?
S6 Zn2 S8 157.56(4) . . ?
C1 S1 Zn1 88.42(12) . . ?
C1 S2 Zn1 81.24(11) . . ?
C6 S3 Zn1 88.58(12) . . ?
C6 S4 Zn1 81.10(12) . . ?
C11 S5 Zn2 85.85(12) . . ?
C11 S6 Zn2 83.13(13) . . ?
C16 S7 Zn2 87.02(13) . . ?
C16 S8 Zn2 82.82(13) . . ?
C1 N1 C2 121.8(3) . . ?
C1 N1 C4 121.8(3) . . ?
C2 N1 C4 116.4(3) . . ?
C6 N2 C7 120.5(3) . . ?
C6 N2 C9 121.9(3) . . ?
C7 N2 C9 117.6(3) . . ?
C11 N3 C14 122.5(3) . . ?
C11 N3 C12 119.5(3) . . ?
C14 N3 C12 117.9(3) . . ?
C16 N4 C17 121.4(3) . . ?
C16 N4 C19 121.1(3) . . ?
C17 N4 C19 117.5(3) . . ?
C25 N5 C21 118.0(3) . . ?
C25 N5 Zn1 121.7(2) . . ?
C21 N5 Zn1 120.3(2) . . ?
C28 N6 C29 117.7(3) . . ?
C28 N6 Zn2 121.8(2) . . ?
C29 N6 Zn2 120.5(2) . . ?
N1 C1 S2 122.4(3) . . ?
N1 C1 S1 120.6(3) . . ?
S2 C1 S1 117.00(19) . . ?
N1 C2 C3 113.1(3) . . ?
O1 C3 C2 113.6(4) . . ?
N1 C4 C5 111.9(3) . . ?
N2 C6 S4 121.2(3) . . ?
N2 C6 S3 121.3(3) . . ?
S4 C6 S3 117.55(19) . . ?
N2 C7 C8 112.2(3) . . ?
O2 C8 C7 112.0(4) . . ?
N2 C9 C10 113.7(3) . . ?
N3 C11 S5 120.5(3) . . ?
N3 C11 S6 122.0(3) . . ?
S5 C11 S6 117.4(2) . . ?
C13 C12 N3 108.1(4) . . ?
O3 C13 C12 110.2(4) . . ?
N3 C14 C15 112.1(4) . . ?
N4 C16 S8 122.7(3) . . ?
N4 C16 S7 120.2(3) . . ?
S8 C16 S7 117.1(2) . . ?
N4 C17 C18 114.6(4) . . ?
O4 C18 C17 111.9(5) . . ?
N4 C19 C20 113.2(4) . . ?
N5 C21 C22 122.7(3) . . ?
C23 C22 C21 119.5(3) . . ?
C22 C23 C24 117.3(3) . . ?
C22 C23 C26 121.1(3) . . ?
C24 C23 C26 121.6(3) . . ?
C25 C24 C23 119.7(3) . . ?
N5 C25 C24 122.8(3) . . ?
C30 C26 C27 117.3(3) . . ?
C30 C26 C23 120.9(3) . . ?
C27 C26 C23 121.8(3) . . ?
C28 C27 C26 119.1(3) . . ?
N6 C28 C27 123.5(3) . . ?
N6 C29 C30 122.7(3) . . ?
C26 C30 C29 119.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N5 2.065(3) . ?
Zn1 S1 2.3397(12) . ?
Zn1 S3 2.3609(11) . ?
Zn1 S2 2.5770(15) . ?
Zn1 S4 2.6056(16) . ?
Zn2 N6 2.082(3) . ?
Zn2 S7 2.3945(12) . ?
Zn2 S5 2.3941(13) . ?
Zn2 S6 2.4908(15) . ?
Zn2 S8 2.5342(16) . ?
S1 C1 1.731(3) . ?
S2 C1 1.720(3) . ?
S3 C6 1.724(3) . ?
S4 C6 1.714(3) . ?
S5 C11 1.720(4) . ?
S6 C11 1.705(4) . ?
S7 C16 1.726(4) . ?
S8 C16 1.716(4) . ?
O1 C3 1.406(5) . ?
O2 C8 1.407(5) . ?
O3 C13 1.450(6) . ?
O4 C18 1.327(7) . ?
N1 C1 1.328(4) . ?
N1 C2 1.476(4) . ?
N1 C4 1.478(4) . ?
N2 C6 1.345(4) . ?
N2 C7 1.475(5) . ?
N2 C9 1.469(5) . ?
N3 C11 1.333(5) . ?
N3 C14 1.464(5) . ?
N3 C12 1.455(5) . ?
N4 C16 1.325(5) . ?
N4 C17 1.471(5) . ?
N4 C19 1.474(5) . ?
N5 C25 1.339(5) . ?
N5 C21 1.338(4) . ?
N6 C28 1.328(5) . ?
N6 C29 1.340(5) . ?
C2 C3 1.513(5) . ?
C4 C5 1.520(6) . ?
C7 C8 1.513(6) . ?
C9 C10 1.508(6) . ?
C12 C13 1.459(7) . ?
C14 C15 1.521(7) . ?
C17 C18 1.494(6) . ?
C19 C20 1.507(8) . ?
C21 C22 1.384(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.393(5) . ?
C23 C26 1.483(5) . ?
C24 C25 1.375(5) . ?
C26 C30 1.397(5) . ?
C26 C27 1.388(5) . ?
C27 C28 1.383(5) . ?
C29 C30 1.375(5) . ?
