#------------------------------------------------------------------------------
#$Date: 2019-11-28 13:32:50 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243872 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/24/7702466.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_7702466
loop_
_publ_author_name
'Rice, Craig R.'
'Wörl, Stefan'
'Jeffery, John C.'
'Paul, Rowena L.'
'Ward, Michael D.'
_publ_section_title
;
 New multidentate ligands for supramolecular coordination chemistry:
 double and triple helical complexes of ligands containing pyridyl and
 thiazolyl donor units
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              550
_journal_paper_doi               10.1039/b007922g
_journal_year                    2001
_chemical_formula_sum            'C52 H42 Cl4 N16 O24 S6 Zn2'
_chemical_formula_weight         1739.92
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 99.357(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.329(3)
_cell_length_b                   23.158(3)
_cell_length_c                   22.379(3)
_cell_measurement_temperature    173(2)
_cell_volume                     6816(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'_diffrn_detector_area_resol_mean  ? '
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21828
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1852P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2630
_reflns_number_gt                5451
_reflns_number_total             7794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007922g.txt
_cod_data_source_block           inxs0
_cod_original_cell_volume        6815.9(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7702466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Zn1 Zn 0.17463(4) 0.12490(2) 0.76521(2) 0.0388(2) Uani 1 1 d .
N11 N 0.0975(3) 0.05139(15) 0.79998(17) 0.0374(8) Uani 1 1 d .
C12 C 0.0279(4) 0.04257(19) 0.8386(2) 0.0411(11) Uani 1 1 d .
C13 C 0.0164(5) -0.0136(2) 0.8544(3) 0.0541(14) Uani 1 1 d .
H13 H -0.0283 -0.0266 0.8794 0.065 Uiso 1 1 calc R
S14 S 0.09731(14) -0.05679(6) 0.82113(8) 0.0606(4) Uani 1 1 d .
C15 C 0.1411(4) 0.00192(19) 0.7879(2) 0.0433(11) Uani 1 1 d .
N21 N 0.2620(3) 0.05305(19) 0.7411(2) 0.0485(10) Uani 1 1 d .
C22 C 0.2239(4) 0.0007(2) 0.7516(2) 0.0451(11) Uani 1 1 d .
C23 C 0.2613(5) -0.0496(2) 0.7305(3) 0.0556(14) Uani 1 1 d .
H23 H 0.2324 -0.0850 0.7373 0.067 Uiso 1 1 calc R
C24 C 0.3415(5) -0.0466(3) 0.6993(3) 0.0686(18) Uani 1 1 d .
H24 H 0.3679 -0.0799 0.6847 0.082 Uiso 1 1 calc R
C25 C 0.3822(5) 0.0065(3) 0.6902(3) 0.0662(17) Uani 1 1 d .
H25 H 0.4376 0.0093 0.6699 0.079 Uiso 1 1 calc R
C26 C 0.3406(4) 0.0559(3) 0.7110(3) 0.0582(14) Uani 1 1 d .
H26 H 0.3680 0.0917 0.7040 0.070 Uiso 1 1 calc R
N31 N 0.0956(3) 0.19604(15) 0.80306(17) 0.0364(8) Uani 1 1 d .
C32 C 0.1388(4) 0.2076(2) 0.8587(2) 0.0458(12) Uani 1 1 d .
S33 S 0.10052(13) 0.27132(6) 0.88742(6) 0.0589(4) Uani 1 1 d .
C34 C 0.0223(4) 0.2836(2) 0.8208(2) 0.0491(12) Uani 1 1 d .
H34 H -0.0187 0.3160 0.8125 0.059 Uiso 1 1 calc R
C35 C 0.0278(4) 0.23915(18) 0.7806(2) 0.0372(10) Uani 1 1 d .
N41 N 0.2581(4) 0.13314(18) 0.8562(2) 0.0535(12) Uani 1 1 d .
C42 C 0.2177(4) 0.1700(2) 0.8916(3) 0.0522(14) Uani 1 1 d .
C43 C 0.2456(6) 0.1716(3) 0.9538(3) 0.074(2) Uani 1 1 d .
H43 H 0.2148 0.1967 0.9777 0.089 Uiso 1 1 calc R
C44 C 0.3224(7) 0.1336(3) 0.9793(3) 0.093(3) Uani 1 1 d .
H44 H 0.3443 0.1340 1.0209 0.111 Uiso 1 1 calc R
C45 C 0.3655(7) 0.0962(3) 0.9442(4) 0.097(3) Uani 1 1 d .
H45 H 0.4159 0.0706 0.9612 0.117 Uiso 1 1 calc R
C46 C 0.3319(5) 0.0973(3) 0.8816(3) 0.0685(19) Uani 1 1 d .
H46 H 0.3616 0.0724 0.8569 0.082 Uiso 1 1 calc R
N51 N -0.0935(3) 0.12585(14) 0.82697(17) 0.0348(8) Uani 1 1 d .
C52 C -0.1291(4) 0.1649(2) 0.8602(2) 0.0425(11) Uani 1 1 d .
S53 S -0.08339(16) 0.16186(7) 0.93615(6) 0.0679(5) Uani 1 1 d .
C54 C -0.0077(6) 0.1050(2) 0.9230(2) 0.0592(16) Uani 1 1 d .
H54 H 0.0378 0.0862 0.9526 0.071 Uiso 1 1 calc R
C55 C -0.0239(4) 0.09105(19) 0.8626(2) 0.0399(10) Uani 1 1 d .
N61 N -0.2504(3) 0.19412(18) 0.7775(2) 0.0474(10) Uani 1 1 d .
C62 C -0.2076(4) 0.2061(2) 0.8334(3) 0.0464(12) Uani 1 1 d .
C63 C -0.2320(6) 0.2545(2) 0.8647(3) 0.0671(18) Uani 1 1 d .
H63 H -0.1990 0.2625 0.9037 0.081 Uiso 1 1 calc R
C64 C -0.3079(6) 0.2905(3) 0.8351(4) 0.079(2) Uani 1 1 d .
H64 H -0.3290 0.3223 0.8552 0.094 Uiso 1 1 calc R
C65 C -0.3514(5) 0.2793(3) 0.7768(4) 0.072(2) Uani 1 1 d .
H65 H -0.4005 0.3039 0.7564 0.086 Uiso 1 1 calc R
C66 C -0.3211(5) 0.2305(3) 0.7482(4) 0.0640(16) Uani 1 1 d .
H66 H -0.3500 0.2228 0.7083 0.077 Uiso 1 1 calc R
Cl1 Cl 0.42147(10) 0.91525(6) 0.89749(6) 0.0510(3) Uani 1 1 d DU
O11A O 0.371(2) 0.8989(10) 0.9422(12) 0.238(17) Uani 0.50 1 d PDU
O11B O 0.436(2) 0.8664(8) 0.9291(10) 0.188(11) Uani 0.50 1 d PU
O12 O 0.5219(5) 0.8959(3) 0.8975(3) 0.111(2) Uani 1 1 d DU
O13A O 0.413(2) 0.9040(7) 0.8350(5) 0.177(10) Uani 0.50 1 d PDU
O13B O 0.3545(11) 0.8824(7) 0.8622(16) 0.210(15) Uani 0.50 1 d PU
O14A O 0.4087(9) 0.9729(4) 0.8837(7) 0.092(4) Uani 0.50 1 d PDU
O14B O 0.4615(12) 0.9645(6) 0.9246(9) 0.135(6) Uani 0.50 1 d PU
Cl2 Cl 0.89175(17) 0.84358(8) 0.90103(8) 0.0785(5) Uani 1 1 d DU
O21 O 0.8652(6) 0.7930(3) 0.9265(5) 0.176(5) Uani 1 1 d DU
O22 O 0.8969(15) 0.8443(5) 0.8441(4) 0.380(15) Uani 1 1 d DU
O23 O 0.9940(8) 0.8549(5) 0.9295(6) 0.243(8) Uani 1 1 d DU
O24 O 0.8441(10) 0.8925(4) 0.9183(5) 0.224(6) Uani 1 1 d DU
O103 O 0.8095(7) 0.0235(5) 0.9097(4) 0.170(4) Uani 1 1 d DU
O104 O 0.8696(15) 0.0050(8) 1.0031(6) 0.408(17) Uani 1 1 d DU
O203 O 0.0135(9) 0.6743(6) 0.8536(5) 0.133(5) Uani 0.643(11) 1 d PDU
O204 O 0.1440(7) 0.6397(3) 0.9109(4) 0.138(3) Uani 1 1 d DU
O205 O 0.2186(16) 0.7026(10) 0.9889(8) 0.114(8) Uani 0.357(11) 1 d PU
C101 C 0.7028(15) 0.0197(10) 0.9774(9) 0.245(13) Uani 1 1 d DU
C201 C 0.0571(10) 0.7101(5) 0.9497(5) 0.123(4) Uani 1 1 d DU
N102 N 0.8050(13) 0.0132(5) 0.9627(4) 0.212(9) Uani 1 1 d DU
N202 N 0.0700(7) 0.6692(4) 0.8998(5) 0.077(3) Uani 0.643(11) 1 d PDU
N206 N 0.149(2) 0.6845(8) 0.9548(10) 0.093(8) Uani 0.357(11) 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
N21 Zn1 N41 95.07(17) . .
N21 Zn1 N51 88.58(16) . 2_556
N41 Zn1 N51 174.25(15) . 2_556
N21 Zn1 N61 98.60(18) . 2_556
N41 Zn1 N61 98.22(19) . 2_556
N51 Zn1 N61 76.81(15) 2_556 2_556
N21 Zn1 N11 78.05(17) . .
N41 Zn1 N11 86.18(17) . .
N51 Zn1 N11 98.94(14) 2_556 .
N61 Zn1 N11 174.74(15) 2_556 .
N21 Zn1 N31 171.94(16) . .
N41 Zn1 N31 77.08(15) . .
N51 Zn1 N31 99.39(14) 2_556 .
N61 Zn1 N31 84.46(16) 2_556 .
N11 Zn1 N31 99.40(15) . .
C15 N11 C12 111.0(4) . .
C15 N11 Zn1 110.5(3) . .
C12 N11 Zn1 137.5(3) . .
C13 C12 N11 114.8(4) . .
C13 C12 C55 123.7(5) . .
N11 C12 C55 121.4(4) . .
C12 C13 S14 109.6(5) . .
C15 S14 C13 90.5(3) . .
N11 C15 C22 121.2(4) . .
N11 C15 S14 114.1(4) . .
C22 C15 S14 124.6(3) . .
C26 N21 C22 118.7(4) . .
C26 N21 Zn1 126.2(4) . .
C22 N21 Zn1 114.6(3) . .
N21 C22 C23 122.1(5) . .
N21 C22 C15 114.6(4) . .
C23 C22 C15 123.3(5) . .
C24 C23 C22 119.2(6) . .
C23 C24 C25 118.8(5) . .
C24 C25 C26 120.0(6) . .
N21 C26 C25 121.3(6) . .
C32 N31 C35 110.9(4) . .
C32 N31 Zn1 110.8(3) . .
C35 N31 Zn1 136.6(3) . .
N31 C32 C42 121.5(4) . .
N31 C32 S33 114.7(4) . .
C42 C32 S33 123.6(4) . .
C34 S33 C32 89.6(2) . .
C35 C34 S33 111.0(4) . .
C34 C35 N31 113.8(4) . .
C34 C35 C35 123.0(4) . 2_556
N31 C35 C35 123.1(3) . 2_556
C42 N41 C46 118.9(5) . .
C42 N41 Zn1 114.8(3) . .
C46 N41 Zn1 125.0(4) . .
N41 C42 C43 123.1(5) . .
N41 C42 C32 114.0(5) . .
C43 C42 C32 122.9(5) . .
C42 C43 C44 117.0(6) . .
C45 C44 C43 121.0(6) . .
C44 C45 C46 118.1(6) . .
N41 C46 C45 121.9(6) . .
C52 N51 C55 110.4(4) . .
C52 N51 Zn1 112.1(3) . 2_556
C55 N51 Zn1 136.7(3) . 2_556
N51 C52 C62 121.2(4) . .
N51 C52 S53 115.6(4) . .
C62 C52 S53 123.2(4) . .
C52 S53 C54 89.2(2) . .
C55 C54 S53 110.3(4) . .
C54 C55 N51 114.5(4) . .
C54 C55 C12 122.2(4) . .
N51 C55 C12 123.3(4) . .
C62 N61 C66 119.3(5) . .
C62 N61 Zn1 114.1(3) . 2_556
C66 N61 Zn1 125.3(5) . 2_556
N61 C62 C63 123.3(5) . .
N61 C62 C52 114.9(4) . .
C63 C62 C52 121.8(5) . .
C62 C63 C64 117.1(7) . .
C65 C64 C63 120.2(6) . .
C64 C65 C66 119.0(6) . .
N61 C66 C65 121.1(7) . .
O13B Cl1 O11B 81.7(13) . .
O13B Cl1 O11A 84.8(19) . .
O11B Cl1 O11A 54.4(15) . .
O13B Cl1 O14B 157.1(10) . .
O11B Cl1 O14B 117.5(12) . .
O11A Cl1 O14B 96.4(16) . .
O13B Cl1 O14A 112.1(10) . .
O11B Cl1 O14A 161.1(13) . .
O11A Cl1 O14A 112.2(11) . .
O14B Cl1 O14A 46.4(8) . .
O13B Cl1 O13A 51.0(15) . .
O11B Cl1 O13A 110.5(12) . .
O11A Cl1 O13A 136(2) . .
O14B Cl1 O13A 124.0(14) . .
O14A Cl1 O13A 88.3(9) . .
O13B Cl1 O12 111.3(11) . .
O11B Cl1 O12 70.8(15) . .
O11A Cl1 O12 120.1(13) . .
O14B Cl1 O12 87.9(7) . .
O14A Cl1 O12 113.1(6) . .
O13A Cl1 O12 82.0(10) . .
O11B O11A Cl1 61.9(10) . .
O11B O11A O13B 66.8(14) . .
Cl1 O11A O13B 47.1(8) . .
O11A O11B Cl1 63.7(13) . .
O11A O11B O12 115.8(16) . .
Cl1 O11B O12 57.0(9) . .
O11A O11B O13B 73(2) . .
Cl1 O11B O13B 49.1(8) . .
O12 O11B O13B 85.5(13) . .
Cl1 O12 O11B 52.2(10) . .
O13B O13A Cl1 61.1(14) . .
O13A O13B Cl1 67.9(10) . .
O13A O13B O11B 99.0(16) . .
Cl1 O13B O11B 49.2(10) . .
O13A O13B O11A 116.0(18) . .
Cl1 O13B O11A 48.1(13) . .
O11B O13B O11A 40.4(13) . .
O14B O14A Cl1 66.1(9) . .
O14A O14B Cl1 67.5(9) . .
O22 Cl2 O21 118.7(7) . .
O22 Cl2 O24 111.5(7) . .
O21 Cl2 O24 114.9(6) . .
O22 Cl2 O23 103.8(9) . .
O21 Cl2 O23 105.2(6) . .
O24 Cl2 O23 99.9(7) . .
N202 O204 N206 70.7(13) . .
N206 C201 N202 64.6(11) . .
O104 N102 O103 129.9(19) . .
O104 N102 C101 116.4(12) . .
O103 N102 C101 113.2(13) . .
O203 N202 O204 128.7(12) . .
O203 N202 C201 117.2(9) . .
O204 N202 C201 113.6(10) . .
O203 N202 N206 160.2(14) . .
O204 N202 N206 61.7(10) . .
C201 N202 N206 53.1(10) . .
O205 N206 C201 120(2) . .
O205 N206 O204 131(3) . .
C201 N206 O204 109(2) . .
O205 N206 N202 166.5(17) . .
C201 N206 N202 62.3(14) . .
O204 N206 N202 47.6(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N21 2.150(4) .
Zn1 N41 2.164(5) .
Zn1 N51 2.168(4) 2_556
Zn1 N61 2.194(4) 2_556
Zn1 N11 2.195(4) .
Zn1 N31 2.198(4) .
N11 C15 1.332(6) .
N11 C12 1.381(7) .
C12 C13 1.364(7) .
C12 C55 1.465(7) .
C13 S14 1.726(6) .
S14 C15 1.698(5) .
C15 C22 1.473(8) .
N21 C26 1.335(8) .
N21 C22 1.350(7) .
C22 C23 1.380(7) .
C23 C24 1.369(9) .
C24 C25 1.373(10) .
C25 C26 1.384(8) .
N31 C32 1.312(6) .
N31 C35 1.385(6) .
C32 C42 1.467(7) .
C32 S33 1.720(5) .
S33 C34 1.699(6) .
C34 C35 1.375(7) .
C35 C35 1.449(9) 2_556
N41 C42 1.336(7) .
N41 C46 1.341(7) .
C42 C43 1.382(8) .
C43 C44 1.399(9) .
C44 C45 1.358(11) .
C45 C46 1.399(9) .
N51 C52 1.308(6) .
N51 C55 1.380(6) .
N51 Zn1 2.168(4) 2_556
C52 C62 1.469(7) .
C52 S53 1.712(5) .
S53 C54 1.714(6) .
C54 C55 1.373(7) .
N61 C62 1.317(7) .
N61 C66 1.352(7) .
N61 Zn1 2.194(4) 2_556
C62 C63 1.388(8) .
C63 C64 1.393(9) .
C64 C65 1.365(11) .
C65 C66 1.389(10) .
Cl1 O13B 1.331(18) .
Cl1 O11B 1.331(17) .
Cl1 O11A 1.352(11) .
Cl1 O14B 1.360(13) .
Cl1 O14A 1.374(8) .
Cl1 O13A 1.408(10) .
Cl1 O12 1.412(6) .
O11A O11B 1.23(3) .
O11A O13B 1.81(4) .
O11B O12 1.59(3) .
O11B O13B 1.74(3) .
O13A O13B 1.18(3) .
O14A O14B 1.078(19) .
Cl2 O22 1.286(10) .
Cl2 O21 1.373(6) .
Cl2 O24 1.384(8) .
Cl2 O23 1.432(9) .
O103 N102 1.221(10) .
O104 N102 1.158(13) .
O203 N202 1.183(11) .
O204 N202 1.193(9) .
O204 N206 1.42(2) .
O205 N206 1.18(3) .
C101 N102 1.460(18) .
C201 N206 1.35(3) .
C201 N202 1.494(14) .
N202 N206 1.52(3) .
