#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:09:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179048 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/10/4301082.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_4301082
loop_
_publ_author_name
'Joachim Ballmann'
'Michael G. G. Fuchs'
'Sebastian Dechert'
'Michael John'
'Franc Meyer'
_publ_contact_author_address
; Institut für Anorganische Chemie
  Georg August Universität Göttingen
  Tammannstraße 4
  D-37077 Göttingen
  Germany
;
_publ_contact_author_email       franc.meyer@chemie.uni-goettingen.de
_publ_contact_author_fax         49(551)393063
_publ_contact_author_name        'Prof. Dr. Franc Meyer'
_publ_contact_author_phone       49(551)393012
_publ_section_title
;
Synthesis and Coordination Properties of Chelating Dithiophenolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              90
_journal_page_last               99
_journal_paper_doi               10.1021/ic801285u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C62 H68 N4 S4 Zn2'
_chemical_formula_sum            'C62 H68 N4 S4 Zn2'
_chemical_formula_weight         1128.18
_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                66.503(3)
_cell_angle_beta                 85.194(4)
_cell_angle_gamma                74.564(4)
_cell_formula_units_Z            1
_cell_length_a                   11.0651(5)
_cell_length_b                   11.7647(5)
_cell_length_c                   12.4259(6)
_cell_measurement_reflns_used    18124
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      1.91
_cell_volume                     1429.48(12)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18124
_diffrn_reflns_theta_full        26.95
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.8639
_exptl_absorpt_correction_T_min  0.7231
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6187
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0269
_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)+(0.0393P)²+0.2833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                5370
_reflns_number_total             6187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801285u_si_003_5.cif
_cod_data_source_block           5d-ab33
_cod_original_cell_volume        1429.48(11)
_cod_database_code               4301082
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 0.046769(16) 0.735804(18) 0.473414(16) 0.01746(6) Uani 1 1 d . . .
S1 S 0.11300(4) 0.62244(4) 0.66121(4) 0.02325(9) Uani 1 1 d . . .
S2 S 0.16429(4) 0.20655(4) 0.55522(4) 0.02347(10) Uani 1 1 d . . .
N1 N 0.12264(12) 0.67595(12) 0.34149(12) 0.0173(3) Uani 1 1 d . . .
N2 N 0.15476(13) 0.86600(13) 0.38806(13) 0.0202(3) Uani 1 1 d . . .
C1 C 0.27946(15) 0.58257(16) 0.65106(14) 0.0209(3) Uani 1 1 d . . .
C2 C 0.34579(16) 0.66473(17) 0.65910(16) 0.0249(3) Uani 1 1 d . . .
H2 H 0.3019 0.7415 0.6643 0.080 Uiso 1 1 calc R . .
C3 C 0.47577(17) 0.63403(19) 0.65941(17) 0.0292(4) Uani 1 1 d . . .
H3 H 0.5183 0.6904 0.6638 0.080 Uiso 1 1 calc R . .
C4 C 0.54180(16) 0.51948(19) 0.65321(18) 0.0307(4) Uani 1 1 d . . .
H4 H 0.6290 0.4968 0.6562 0.080 Uiso 1 1 calc R . .
C5 C 0.47725(17) 0.43875(18) 0.64249(17) 0.0287(4) Uani 1 1 d . . .
H5 H 0.5223 0.3625 0.6368 0.080 Uiso 1 1 calc R . .
C6 C 0.34630(16) 0.46830(16) 0.63990(15) 0.0228(3) Uani 1 1 d . . .
C7 C 0.28234(17) 0.38239(17) 0.61557(16) 0.0258(4) Uani 1 1 d . . .
H7A H 0.3411 0.3360 0.5756 0.080 Uiso 1 1 calc R . .
H7B H 0.2125 0.4366 0.5613 0.080 Uiso 1 1 calc R . .
C8 C 0.23314(15) 0.28540(16) 0.71921(15) 0.0211(3) Uani 1 1 d . . .
C10 C 0.23930(16) 0.27889(16) 0.83292(16) 0.0245(3) Uani 1 1 d . . .
H10 H 0.2768 0.3340 0.8466 0.080 Uiso 1 1 calc R . .
C11 C 0.19056(17) 0.19159(17) 0.92670(16) 0.0273(4) Uani 1 1 d . . .
H11 H 0.1942 0.1897 1.0019 0.080 Uiso 1 1 calc R . .
C12 C 0.13673(17) 0.10756(17) 0.90742(17) 0.0273(4) Uani 1 1 d . . .
H12 H 0.1050 0.0482 0.9698 0.080 Uiso 1 1 calc R . .
C13 C 0.13039(16) 0.11229(16) 0.79468(17) 0.0248(4) Uani 1 1 d . . .
H13 H 0.0945 0.0554 0.7822 0.080 Uiso 1 1 calc R . .
C14 C 0.17692(15) 0.20091(15) 0.69933(15) 0.0206(3) Uani 1 1 d . . .
C15 C 0.08688(15) 0.58993(15) 0.31502(15) 0.0203(3) Uani 1 1 d . . .
H15 H 0.0427 0.5367 0.3701 0.080 Uiso 1 1 calc R . .
C16 C 0.11276(15) 0.57680(15) 0.20961(15) 0.0207(3) Uani 1 1 d . . .
H16 H 0.0861 0.5156 0.1949 0.080 Uiso 1 1 calc R . .
C17 C 0.17884(15) 0.65501(15) 0.12477(15) 0.0190(3) Uani 1 1 d . A .
C18 C 0.21701(15) 0.74372(15) 0.15428(15) 0.0196(3) Uani 1 1 d . . .
H18 H 0.2626 0.7971 0.1013 0.080 Uiso 1 1 calc R . .
C19 C 0.18738(14) 0.75250(14) 0.26154(14) 0.0175(3) Uani 1 1 d . . .
C20 C 0.21900(14) 0.84829(14) 0.29718(14) 0.0179(3) Uani 1 1 d . . .
C21 C 0.31003(15) 0.91355(15) 0.24238(14) 0.0191(3) Uani 1 1 d . . .
H21 H 0.3531 0.8993 0.1795 0.080 Uiso 1 1 calc R . .
C22 C 0.33637(15) 1.00001(15) 0.28179(15) 0.0192(3) Uani 1 1 d . . .
C23 C 0.26750(16) 1.01775(16) 0.37561(16) 0.0241(3) Uani 1 1 d . . .
H23 H 0.2811 1.0755 0.4041 0.080 Uiso 1 1 calc R . .
C24 C 0.17935(16) 0.94971(17) 0.42620(16) 0.0243(3) Uani 1 1 d . . .
H24 H 0.1351 0.9622 0.4893 0.080 Uiso 1 1 calc R . .
C25 C 0.20816(16) 0.64637(16) 0.00585(15) 0.0241(3) Uani 1 1 d D . .
C26A C 0.1459(2) 0.5528(2) -0.01115(19) 0.0339(5) Uani 0.894(2) 1 d PD A 1
H26A H 0.1739 0.4695 0.0504 0.080 Uiso 0.894(2) 1 calc PR A 1
H26B H 0.1682 0.5478 -0.0857 0.080 Uiso 0.894(2) 1 calc PR A 1
H26C H 0.0565 0.5825 -0.0087 0.080 Uiso 0.894(2) 1 calc PR A 1
C27A C 0.3517(2) 0.5969(2) 0.0009(2) 0.0344(5) Uani 0.894(2) 1 d PD A 1
H27A H 0.3793 0.5134 0.0622 0.080 Uiso 0.894(2) 1 calc PR A 1
H27B H 0.3922 0.6547 0.0114 0.080 Uiso 0.894(2) 1 calc PR A 1
H27C H 0.3729 0.5920 -0.0739 0.080 Uiso 0.894(2) 1 calc PR A 1
C28A C 0.1632(2) 0.77805(19) -0.09092(18) 0.0330(5) Uani 0.894(2) 1 d PD A 1
H28A H 0.1812 0.7725 -0.1659 0.080 Uiso 0.894(2) 1 calc PR A 1
H28B H 0.2054 0.8357 -0.0827 0.080 Uiso 0.894(2) 1 calc PR A 1
H28C H 0.0744 0.8093 -0.0855 0.080 Uiso 0.894(2) 1 calc PR A 1
C26B C 0.3050(11) 0.7227(12) -0.0635(13) 0.0339(5) Uani 0.106(2) 1 d PD A 2
H26D H 0.3199 0.7140 -0.1374 0.080 Uiso 0.106(2) 1 calc PR A 2
H26E H 0.3823 0.6893 -0.0187 0.080 Uiso 0.106(2) 1 calc PR A 2
H26F H 0.2723 0.8115 -0.0769 0.080 Uiso 0.106(2) 1 calc PR A 2
C27B C 0.0832(9) 0.7193(13) -0.0701(13) 0.0344(5) Uani 0.106(2) 1 d PD A 2
H27D H 0.0959 0.7167 -0.1465 0.080 Uiso 0.106(2) 1 calc PR A 2
H27E H 0.0598 0.8069 -0.0776 0.080 Uiso 0.106(2) 1 calc PR A 2
H27F H 0.0176 0.6788 -0.0323 0.080 Uiso 0.106(2) 1 calc PR A 2
C28B C 0.2488(13) 0.5138(8) 0.0023(14) 0.0330(5) Uani 0.106(2) 1 d PD A 2
H28D H 0.2649 0.5219 -0.0772 0.080 Uiso 0.106(2) 1 calc PR A 2
H28E H 0.1833 0.4705 0.0322 0.080 Uiso 0.106(2) 1 calc PR A 2
H28F H 0.3237 0.4653 0.0497 0.080 Uiso 0.106(2) 1 calc PR A 2
C29 C 0.43694(15) 1.07238(15) 0.22860(15) 0.0208(3) Uani 1 1 d . . .
C30 C 0.50382(17) 1.03907(18) 0.12850(17) 0.0277(4) Uani 1 1 d . . .
H30A H 0.4438 1.0602 0.0676 0.080 Uiso 1 1 calc R . .
H30B H 0.5441 0.9490 0.1574 0.080 Uiso 1 1 calc R . .
H30C H 0.5656 1.0870 0.0975 0.080 Uiso 1 1 calc R . .
C31 C 0.37442(17) 1.21698(16) 0.18111(17) 0.0277(4) Uani 1 1 d . . .
H31A H 0.3164 1.2389 0.1184 0.080 Uiso 1 1 calc R . .
H31B H 0.4375 1.2636 0.1523 0.080 Uiso 1 1 calc R . .
H31C H 0.3304 1.2387 0.2430 0.080 Uiso 1 1 calc R . .
C32 C 0.53397(17) 1.03787(18) 0.32591(17) 0.0286(4) Uani 1 1 d . . .
H32A H 0.6000 1.0796 0.2931 0.080 Uiso 1 1 calc R . .
H32B H 0.5685 0.9467 0.3594 0.080 Uiso 1 1 calc R . .
H32C H 0.4939 1.0658 0.3859 0.080 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'
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
N1 Zn1 N2 78.78(5) . . ?
N1 Zn1 S1 121.54(4) . . ?
N2 Zn1 S1 110.06(4) . . ?
N1 Zn1 S2 106.29(4) . 2_566 ?
N2 Zn1 S2 121.03(4) . 2_566 ?
S1 Zn1 S2 114.877(18) . 2_566 ?
C1 S1 Zn1 103.27(6) . . ?
C14 S2 Zn1 101.46(5) . 2_566 ?
C15 N1 C19 118.44(14) . . ?
C15 N1 Zn1 124.21(11) . . ?
C19 N1 Zn1 115.16(10) . . ?
C20 N2 C24 118.38(14) . . ?
C20 N2 Zn1 114.76(10) . . ?
C24 N2 Zn1 126.04(11) . . ?
C2 C1 C6 119.02(15) . . ?
C2 C1 S1 119.05(13) . . ?
C6 C1 S1 121.88(13) . . ?
C3 C2 C1 121.30(16) . . ?
C4 C3 C2 119.81(17) . . ?
C3 C4 C5 119.43(16) . . ?
C4 C5 C6 121.94(17) . . ?
C5 C6 C1 118.42(15) . . ?
C5 C6 C7 118.88(15) . . ?
C1 C6 C7 122.50(15) . . ?
C6 C7 C8 117.81(15) . . ?
C10 C8 C14 118.92(16) . . ?
C10 C8 C7 122.12(15) . . ?
C14 C8 C7 118.94(15) . . ?
C8 C10 C11 121.42(16) . . ?
C12 C11 C10 119.65(17) . . ?
C11 C12 C13 119.68(17) . . ?
C12 C13 C14 121.32(16) . . ?
C13 C14 C8 118.99(16) . . ?
C13 C14 S2 120.14(13) . . ?
C8 C14 S2 120.88(13) . . ?
N1 C15 C16 122.78(15) . . ?
C15 C16 C17 120.20(14) . . ?
C16 C17 C18 116.38(15) . . ?
C16 C17 C25 122.50(14) . . ?
C18 C17 C25 121.12(14) . . ?
C19 C18 C17 120.53(15) . . ?
N1 C19 C18 121.66(14) . . ?
N1 C19 C20 114.50(14) . . ?
C18 C19 C20 123.81(14) . . ?
N2 C20 C21 121.91(14) . . ?
N2 C20 C19 114.96(13) . . ?
C21 C20 C19 123.12(14) . . ?
C22 C21 C20 120.01(15) . . ?
C21 C22 C23 117.02(15) . . ?
C21 C22 C29 123.12(15) . . ?
C23 C22 C29 119.86(14) . . ?
C24 C23 C22 120.05(15) . . ?
N2 C24 C23 122.63(15) . . ?
C28A C25 C28B 131.2(6) . . ?
C28A C25 C17 109.48(14) . . ?
C28B C25 C17 118.0(6) . . ?
C28A C25 C26A 109.40(16) . . ?
C17 C25 C26A 111.65(15) . . ?
C28A C25 C27A 110.04(16) . . ?
C17 C25 C27A 107.78(15) . . ?
C26A C25 C27A 108.47(15) . . ?
C28B C25 C26B 108.0(6) . . ?
C17 C25 C26B 113.0(6) . . ?
C28B C25 C27B 107.0(6) . . ?
C17 C25 C27B 105.7(6) . . ?
C27A C25 C27B 144.6(6) . . ?
C26B C25 C27B 104.2(5) . . ?
C30 C29 C22 112.39(13) . . ?
C30 C29 C31 108.73(15) . . ?
C22 C29 C31 108.64(13) . . ?
C30 C29 C32 109.03(14) . . ?
C22 C29 C32 108.43(14) . . ?
C31 C29 C32 109.58(14) . . ?
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 N1 2.0647(13) . ?
Zn1 N2 2.0894(14) . ?
Zn1 S1 2.2463(5) . ?
Zn1 S2 2.2681(4) 2_566 ?
Zn1 Zn1 5.6843(4) 2_566 ?
S1 C1 1.7823(16) . ?
S2 C14 1.7813(17) . ?
S2 Zn1 2.2681(4) 2_566 ?
N1 C15 1.338(2) . ?
N1 C19 1.350(2) . ?
N2 C20 1.341(2) . ?
N2 C24 1.343(2) . ?
C1 C2 1.396(2) . ?
C1 C6 1.406(2) . ?
C2 C3 1.386(2) . ?
C3 C4 1.380(3) . ?
C4 C5 1.381(3) . ?
C5 C6 1.397(2) . ?
C6 C7 1.508(2) . ?
C7 C8 1.516(2) . ?
C8 C10 1.391(2) . ?
C8 C14 1.410(2) . ?
C10 C11 1.392(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.398(2) . ?
C15 C16 1.377(2) . ?
C16 C17 1.396(2) . ?
C17 C18 1.403(2) . ?
C17 C25 1.524(2) . ?
C18 C19 1.383(2) . ?
C19 C20 1.491(2) . ?
C20 C21 1.396(2) . ?
C21 C22 1.392(2) . ?
C22 C23 1.394(2) . ?
C22 C29 1.527(2) . ?
C23 C24 1.378(2) . ?
C25 C28A 1.516(2) . ?
C25 C28B 1.521(7) . ?
C25 C26A 1.531(2) . ?
C25 C27A 1.545(3) . ?
C25 C26B 1.561(7) . ?
C25 C27B 1.575(7) . ?
C29 C30 1.526(2) . ?
C29 C31 1.537(2) . ?
C29 C32 1.541(2) . ?
