#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:09:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179048 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/10/4301080.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_4301080
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         'C60 H56 Cl8 N4 S4 Zn2, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H60 Cl12 N4 S4 Zn2'
_chemical_formula_weight         1545.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.274(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7471(6)
_cell_length_b                   11.0026(2)
_cell_length_c                   18.2732(7)
_cell_measurement_reflns_used    39436
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.03
_cell_volume                     3301.86(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'X-RED (Stoe & Cie, 2002)'
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39436
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.8933
_exptl_absorpt_correction_T_min  0.7558
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7170
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0373
_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)+(0.0441P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                5722
_reflns_number_total             7170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801285u_si_003_3.cif
_cod_data_source_block           5a-ab35
_cod_original_cell_volume        3301.86(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301080
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.405053(16) 0.40737(3) 0.453562(16) 0.01671(7) Uani 1 1 d . . .
S1 S 0.46885(3) 0.60903(6) 0.43483(3) 0.01663(12) Uani 1 1 d . . .
S2 S 0.41431(4) 0.32382(6) 0.34147(3) 0.01919(13) Uani 1 1 d . . .
N1 N 0.28905(12) 0.4859(2) 0.42301(11) 0.0179(4) Uani 1 1 d . . .
N2 N 0.34507(12) 0.28900(19) 0.50827(12) 0.0168(4) Uani 1 1 d . . .
Cl1 Cl 0.38875(4) 0.83203(6) 0.32290(4) 0.02934(15) Uani 1 1 d . . .
Cl2 Cl 0.50065(5) 0.68301(8) 0.10516(4) 0.04026(19) Uani 1 1 d . . .
Cl3 Cl 0.79309(4) 0.30818(8) 0.42737(4) 0.03525(17) Uani 1 1 d . . .
Cl4 Cl 0.52514(5) 0.10745(6) 0.44357(4) 0.03081(15) Uani 1 1 d . . .
C1 C 0.47721(14) 0.6221(2) 0.34194(14) 0.0177(5) Uani 1 1 d . . .
C2 C 0.44084(15) 0.7212(2) 0.29306(15) 0.0205(5) Uani 1 1 d . . .
C3 C 0.44610(17) 0.7406(3) 0.22009(16) 0.0262(6) Uani 1 1 d . . .
H3 H 0.4205 0.8067 0.1888 0.080 Uiso 1 1 calc R . .
C4 C 0.49059(17) 0.6587(3) 0.19533(15) 0.0257(6) Uani 1 1 d . . .
C5 C 0.52617(16) 0.5582(2) 0.24025(15) 0.0231(5) Uani 1 1 d . . .
H5 H 0.5550 0.5036 0.2220 0.080 Uiso 1 1 calc R . .
C6 C 0.51926(14) 0.5376(2) 0.31333(14) 0.0176(5) Uani 1 1 d . . .
C7 C 0.56286(15) 0.4279(2) 0.35771(13) 0.0179(5) Uani 1 1 d . . .
C8 C 0.64640(15) 0.4212(3) 0.37470(14) 0.0220(5) Uani 1 1 d . . .
H8 H 0.6728 0.4852 0.3612 0.080 Uiso 1 1 calc R . .
C9 C 0.69014(16) 0.3188(3) 0.41189(15) 0.0246(5) Uani 1 1 d . . .
C10 C 0.65342(17) 0.2245(3) 0.43508(15) 0.0263(6) Uani 1 1 d . . .
H10 H 0.6836 0.1582 0.4623 0.080 Uiso 1 1 calc R . .
C11 C 0.57007(17) 0.2307(2) 0.41680(15) 0.0229(5) Uani 1 1 d . . .
C12 C 0.52139(15) 0.3293(2) 0.37535(14) 0.0187(5) Uani 1 1 d . . .
C13 C 0.26087(15) 0.5776(2) 0.37141(15) 0.0229(5) Uani 1 1 d . . .
H13 H 0.2960 0.6145 0.3512 0.080 Uiso 1 1 calc R . .
C14 C 0.18164(15) 0.6194(3) 0.34706(15) 0.0232(5) Uani 1 1 d . . .
H14 H 0.1641 0.6820 0.3103 0.080 Uiso 1 1 calc R . .
C15 C 0.12787(14) 0.5677(2) 0.37770(14) 0.0183(5) Uani 1 1 d . . .
C16 C 0.15794(14) 0.4717(2) 0.43069(14) 0.0182(5) Uani 1 1 d . . .
H16 H 0.1243 0.4335 0.4521 0.080 Uiso 1 1 calc R . .
C17 C 0.23780(14) 0.4328(2) 0.45164(13) 0.0150(4) Uani 1 1 d . . .
C18 C 0.27248(14) 0.3287(2) 0.50616(13) 0.0154(4) Uani 1 1 d . . .
C19 C 0.23522(15) 0.2778(2) 0.55300(14) 0.0190(5) Uani 1 1 d . . .
H19 H 0.1857 0.3087 0.5511 0.080 Uiso 1 1 calc R . .
C20 C 0.27145(15) 0.1802(2) 0.60334(14) 0.0196(5) Uani 1 1 d . A .
C21 C 0.34479(15) 0.1380(2) 0.60229(15) 0.0205(5) Uani 1 1 d . . .
H21 H 0.3707 0.0721 0.6336 0.080 Uiso 1 1 calc R . .
C22 C 0.37949(15) 0.1939(2) 0.55469(14) 0.0195(5) Uani 1 1 d . . .
H22 H 0.4287 0.1642 0.5550 0.080 Uiso 1 1 calc R . .
C23 C 0.04067(15) 0.6142(2) 0.35159(15) 0.0223(5) Uani 1 1 d . . .
C24 C 0.04049(18) 0.7526(3) 0.35873(19) 0.0324(6) Uani 1 1 d . . .
H24A H 0.0707 0.7758 0.4126 0.080 Uiso 1 1 calc R . .
H24B H -0.0146 0.7810 0.3428 0.080 Uiso 1 1 calc R . .
H24C H 0.0653 0.7880 0.3253 0.080 Uiso 1 1 calc R . .
C25 C -0.00406(17) 0.5789(3) 0.26431(17) 0.0311(6) Uani 1 1 d . . .
H25A H 0.0253 0.6099 0.2337 0.080 Uiso 1 1 calc R . .
H25B H -0.0579 0.6128 0.2450 0.080 Uiso 1 1 calc R . .
H25C H -0.0075 0.4920 0.2597 0.080 Uiso 1 1 calc R . .
C26 C -0.00380(17) 0.5593(3) 0.40132(18) 0.0325(7) Uani 1 1 d . . .
H26A H -0.0054 0.4725 0.3960 0.080 Uiso 1 1 calc R . .
H26B H -0.0584 0.5905 0.3832 0.080 Uiso 1 1 calc R . .
H26C H 0.0246 0.5807 0.4559 0.080 Uiso 1 1 calc R . .
C27 C 0.23015(17) 0.1260(2) 0.65546(16) 0.0284(6) Uani 1 1 d D . .
C28A C 0.2161(2) 0.2260(3) 0.70642(19) 0.0320(7) Uani 0.892(4) 1 d PD A 1
H28A H 0.1859 0.2911 0.6732 0.080 Uiso 0.892(4) 1 calc PR A 1
H28B H 0.2676 0.2561 0.7424 0.080 Uiso 0.892(4) 1 calc PR A 1
H28C H 0.1858 0.1939 0.7359 0.080 Uiso 0.892(4) 1 calc PR A 1
C29A C 0.1454(2) 0.0758(4) 0.6007(2) 0.0415(9) Uani 0.892(4) 1 d PD A 1
H29A H 0.1141 0.1399 0.5672 0.080 Uiso 0.892(4) 1 calc PR A 1
H29B H 0.1171 0.0454 0.6325 0.080 Uiso 0.892(4) 1 calc PR A 1
H29C H 0.1526 0.0113 0.5686 0.080 Uiso 0.892(4) 1 calc PR A 1
C30A C 0.2777(3) 0.0232(4) 0.7072(2) 0.0464(10) Uani 0.892(4) 1 d PD A 1
H30A H 0.2488 -0.0069 0.7384 0.080 Uiso 0.892(4) 1 calc PR A 1
H30B H 0.3303 0.0523 0.7414 0.080 Uiso 0.892(4) 1 calc PR A 1
H30C H 0.2842 -0.0410 0.6745 0.080 Uiso 0.892(4) 1 calc PR A 1
C28B C 0.2142(14) -0.0090(9) 0.6396(14) 0.0320(7) Uani 0.108(4) 1 d PD A 2
H28D H 0.2598 -0.0459 0.6322 0.080 Uiso 0.108(4) 1 calc PR A 2
H28E H 0.1661 -0.0201 0.5928 0.080 Uiso 0.108(4) 1 calc PR A 2
H28F H 0.2065 -0.0463 0.6838 0.080 Uiso 0.108(4) 1 calc PR A 2
C29B C 0.3028(11) 0.138(2) 0.7361(9) 0.0415(9) Uani 0.108(4) 1 d PD A 2
H29D H 0.3486 0.0936 0.7343 0.080 Uiso 0.108(4) 1 calc PR A 2
H29E H 0.2875 0.1060 0.7773 0.080 Uiso 0.108(4) 1 calc PR A 2
H29F H 0.3172 0.2223 0.7464 0.080 Uiso 0.108(4) 1 calc PR A 2
C30B C 0.1587(11) 0.193(2) 0.6621(16) 0.0464(10) Uani 0.108(4) 1 d PD A 2
H30D H 0.1732 0.2770 0.6748 0.080 Uiso 0.108(4) 1 calc PR A 2
H30E H 0.1446 0.1572 0.7030 0.080 Uiso 0.108(4) 1 calc PR A 2
H30F H 0.1130 0.1887 0.6127 0.080 Uiso 0.108(4) 1 calc PR A 2
C31 C 0.7124(2) 0.5129(3) 0.8412(2) 0.0435(8) Uani 1 1 d . . .
H31A H 0.7348 0.5932 0.8409 0.080 Uiso 1 1 calc R . .
H31B H 0.6631 0.5051 0.7941 0.080 Uiso 1 1 calc R . .
Cl5 Cl 0.78328(5) 0.40233(8) 0.83921(5) 0.04261(19) Uani 1 1 d . . .
Cl6 Cl 0.68817(5) 0.49692(8) 0.92554(4) 0.04099(19) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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 76.44(8) . . ?
N1 Zn1 S2 108.66(6) . . ?
N2 Zn1 S2 112.66(6) . . ?
N1 Zn1 S1 139.57(6) . 3_666 ?
N2 Zn1 S1 91.48(5) . 3_666 ?
S2 Zn1 S1 111.59(2) . 3_666 ?
N1 Zn1 S1 92.64(6) . . ?
N2 Zn1 S1 154.64(6) . . ?
S2 Zn1 S1 92.43(2) . . ?
S1 Zn1 S1 82.07(2) 3_666 . ?
C1 S1 Zn1 115.65(8) . 3_666 ?
C1 S1 Zn1 113.59(8) . . ?
Zn1 S1 Zn1 97.93(2) 3_666 . ?
C12 S2 Zn1 96.01(8) . . ?
C13 N1 C17 118.3(2) . . ?
C13 N1 Zn1 124.21(17) . . ?
C17 N1 Zn1 117.16(16) . . ?
C22 N2 C18 118.2(2) . . ?
C22 N2 Zn1 125.42(16) . . ?
C18 N2 Zn1 115.25(16) . . ?
C2 C1 C6 117.2(2) . . ?
C2 C1 S1 119.33(19) . . ?
C6 C1 S1 123.49(19) . . ?
C3 C2 C1 123.3(2) . . ?
C3 C2 Cl1 115.5(2) . . ?
C1 C2 Cl1 121.1(2) . . ?
C4 C3 C2 118.0(2) . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 Cl2 119.8(2) . . ?
C3 C4 Cl2 119.0(2) . . ?
C4 C5 C6 120.7(2) . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C7 115.6(2) . . ?
C1 C6 C7 124.6(2) . . ?
C8 C7 C12 120.6(2) . . ?
C8 C7 C6 116.8(2) . . ?
C12 C7 C6 122.4(2) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 121.3(2) . . ?
C10 C9 Cl3 119.3(2) . . ?
C8 C9 Cl3 119.3(2) . . ?
C9 C10 C11 118.3(2) . . ?
C10 C11 C12 123.1(3) . . ?
C10 C11 Cl4 117.0(2) . . ?
C12 C11 Cl4 119.8(2) . . ?
C11 C12 C7 116.4(2) . . ?
C11 C12 S2 121.4(2) . . ?
C7 C12 S2 122.06(19) . . ?
N1 C13 C14 122.6(2) . . ?
C13 C14 C15 120.1(2) . . ?
C16 C15 C14 116.5(2) . . ?
C16 C15 C23 123.2(2) . . ?
C14 C15 C23 120.3(2) . . ?
C17 C16 C15 120.4(2) . . ?
N1 C17 C16 122.0(2) . . ?
N1 C17 C18 115.2(2) . . ?
C16 C17 C18 122.8(2) . . ?
N2 C18 C19 121.9(2) . . ?
N2 C18 C17 114.6(2) . . ?
C19 C18 C17 123.5(2) . . ?
C18 C19 C20 120.5(2) . . ?
C21 C20 C19 116.5(2) . . ?
C21 C20 C27 123.5(2) . . ?
C19 C20 C27 120.0(2) . . ?
C22 C21 C20 120.1(2) . . ?
N2 C22 C21 122.7(2) . . ?
C15 C23 C24 110.0(2) . . ?
C15 C23 C26 111.8(2) . . ?
C24 C23 C26 108.9(2) . . ?
C15 C23 C25 107.7(2) . . ?
C24 C23 C25 108.9(2) . . ?
C26 C23 C25 109.6(2) . . ?
C30B C27 C28B 113.1(10) . . ?
C30A C27 C28A 109.9(3) . . ?
C28B C27 C28A 139.6(9) . . ?
C30A C27 C20 113.4(2) . . ?
C30B C27 C20 118.3(10) . . ?
C28B C27 C20 111.2(9) . . ?
C28A C27 C20 109.2(2) . . ?
C30B C27 C29B 107.5(9) . . ?
C28B C27 C29B 107.0(9) . . ?
C20 C27 C29B 97.8(10) . . ?
C30A C27 C29A 108.1(3) . . ?
C30B C27 C29A 65.8(10) . . ?
C28B C27 C29A 57.7(9) . . ?
C28A C27 C29A 107.9(3) . . ?
C20 C27 C29A 108.3(2) . . ?
Cl6 C31 Cl5 111.29(18) . . ?
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 2.104(2) . ?
Zn1 N2 2.153(2) . ?
Zn1 S2 2.3071(6) . ?
Zn1 S1 2.3959(6) 3_666 ?
Zn1 S1 2.5721(7) . ?
Zn1 Zn1 3.7493(6) 3_666 ?
S1 C1 1.765(2) . ?
S1 Zn1 2.3959(6) 3_666 ?
S2 C12 1.763(3) . ?
N1 C13 1.341(3) . ?
N1 C17 1.343(3) . ?
N2 C22 1.340(3) . ?
N2 C18 1.347(3) . ?
Cl1 C2 1.738(3) . ?
Cl2 C4 1.744(3) . ?
Cl3 C9 1.743(3) . ?
Cl4 C11 1.735(3) . ?
C1 C2 1.402(3) . ?
C1 C6 1.411(4) . ?
C2 C3 1.388(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.405(3) . ?
C6 C7 1.496(3) . ?
C7 C8 1.397(3) . ?
C7 C12 1.415(4) . ?
C8 C9 1.391(4) . ?
C9 C10 1.375(4) . ?
C10 C11 1.389(4) . ?
C11 C12 1.414(4) . ?
C13 C14 1.383(4) . ?
C14 C15 1.397(4) . ?
C15 C16 1.395(3) . ?
C15 C23 1.525(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.489(3) . ?
C18 C19 1.383(3) . ?
C19 C20 1.402(4) . ?
C20 C21 1.389(4) . ?
C20 C27 1.526(4) . ?
C21 C22 1.386(4) . ?
C23 C24 1.529(4) . ?
C23 C26 1.535(4) . ?
C23 C25 1.538(4) . ?
C27 C30A 1.510(4) . ?
C27 C30B 1.513(8) . ?
C27 C28B 1.519(8) . ?
C27 C28A 1.522(4) . ?
C27 C29B 1.552(8) . ?
C27 C29A 1.559(4) . ?
C31 Cl6 1.759(4) . ?
C31 Cl5 1.760(4) . ?
