#------------------------------------------------------------------------------
#$Date: 2019-11-28 13:32:50 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243872 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/24/7702467.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_7702467
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 Co2 N16 O24 S6'
_chemical_formula_weight         1727.04
_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                 99.8610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2594(7)
_cell_length_b                   23.1248(12)
_cell_length_c                   22.4373(11)
_cell_measurement_temperature    173(2)
_cell_volume                     6778.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21778
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.1011
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3078
_refine_ls_wR_factor_ref         0.3315
_reflns_number_gt                4840
_reflns_number_total             7757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007922g.txt
_cod_data_source_block           girlfrim
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7702467
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
Co1 Co 0.17168(6) 0.12591(3) 0.76601(4) 0.0406(3) Uani 1 1 d .
S14 S 0.09776(17) -0.05585(7) 0.82097(9) 0.0607(5) Uani 1 1 d .
S33 S 0.10044(17) 0.27130(8) 0.88772(9) 0.0621(6) Uani 1 1 d .
S53 S -0.0849(2) 0.16293(9) 0.93444(9) 0.0734(7) Uani 1 1 d .
N11 N 0.0980(4) 0.0524(2) 0.7997(2) 0.0417(12) Uani 1 1 d .
N21 N 0.2580(4) 0.0552(2) 0.7404(3) 0.0505(14) Uani 1 1 d .
N31 N 0.0955(4) 0.1958(2) 0.8033(2) 0.0395(11) Uani 1 1 d .
N41 N 0.2546(5) 0.1322(2) 0.8563(3) 0.0583(16) Uani 1 1 d .
N51 N -0.0928(4) 0.12700(19) 0.8257(2) 0.0375(11) Uani 1 1 d .
N61 N -0.2476(4) 0.1956(2) 0.7747(3) 0.0542(15) Uani 1 1 d .
C12 C 0.0288(5) 0.0435(2) 0.8381(3) 0.0410(14) Uani 1 1 d .
C13 C 0.0169(6) -0.0127(3) 0.8546(3) 0.0556(18) Uani 1 1 d .
H13 H -0.0273 -0.0256 0.8798 0.067 Uiso 1 1 calc R
C15 C 0.1411(5) 0.0028(3) 0.7877(3) 0.0451(15) Uani 1 1 d .
C22 C 0.2227(5) 0.0021(3) 0.7510(3) 0.0494(16) Uani 1 1 d .
C23 C 0.2601(6) -0.0477(3) 0.7304(3) 0.0596(19) Uani 1 1 d .
H23 H 0.2324 -0.0835 0.7375 0.071 Uiso 1 1 calc R
C24 C 0.3417(7) -0.0433(4) 0.6980(4) 0.070(2) Uani 1 1 d .
H24 H 0.3686 -0.0760 0.6823 0.084 Uiso 1 1 calc R
C25 C 0.3798(7) 0.0096(4) 0.6904(4) 0.071(2) Uani 1 1 d .
H25 H 0.4374 0.0133 0.6722 0.085 Uiso 1 1 calc R
C26 C 0.3344(6) 0.0588(4) 0.7092(4) 0.067(2) Uani 1 1 d .
H26 H 0.3579 0.0950 0.6999 0.080 Uiso 1 1 calc R
C32 C 0.1384(6) 0.2078(3) 0.8594(3) 0.0493(16) Uani 1 1 d .
C34 C 0.0220(6) 0.2836(3) 0.8204(3) 0.0502(16) Uani 1 1 d .
H34 H -0.0193 0.3161 0.8118 0.060 Uiso 1 1 calc R
C35 C 0.0278(5) 0.2396(2) 0.7809(3) 0.0403(13) Uani 1 1 d .
C42 C 0.2180(6) 0.1692(3) 0.8921(3) 0.0565(18) Uani 1 1 d .
C43 C 0.2483(8) 0.1720(3) 0.9532(4) 0.084(3) Uani 1 1 d .
H43 H 0.2200 0.1988 0.9765 0.100 Uiso 1 1 calc R
C44 C 0.3235(10) 0.1329(4) 0.9798(5) 0.125(6) Uani 1 1 d .
H44 H 0.3459 0.1329 1.0214 0.150 Uiso 1 1 calc R
C45 C 0.3635(9) 0.0948(4) 0.9435(5) 0.112(5) Uani 1 1 d .
H45 H 0.4130 0.0683 0.9603 0.135 Uiso 1 1 calc R
C46 C 0.3297(7) 0.0958(4) 0.8811(4) 0.078(3) Uani 1 1 d .
H46 H 0.3594 0.0711 0.8563 0.094 Uiso 1 1 calc R
C52 C -0.1298(5) 0.1663(3) 0.8590(3) 0.0466(15) Uani 1 1 d .
C54 C -0.0065(7) 0.1058(3) 0.9220(3) 0.060(2) Uani 1 1 d .
H54 H 0.0403 0.0877 0.9518 0.072 Uiso 1 1 calc R
C55 C -0.0233(5) 0.0914(3) 0.8623(3) 0.0442(14) Uani 1 1 d .
C62 C -0.2074(6) 0.2073(3) 0.8314(3) 0.0508(16) Uani 1 1 d .
C63 C -0.2373(8) 0.2539(3) 0.8608(5) 0.078(3) Uani 1 1 d .
H63 H -0.2070 0.2609 0.9007 0.093 Uiso 1 1 calc R
C64 C -0.3118(8) 0.2909(4) 0.8324(5) 0.085(3) Uani 1 1 d .
H64 H -0.3346 0.3222 0.8525 0.102 Uiso 1 1 calc R
C65 C -0.3501(7) 0.2794(4) 0.7736(6) 0.088(3) Uani 1 1 d .
H65 H -0.3992 0.3039 0.7524 0.105 Uiso 1 1 calc R
C66 C -0.3179(6) 0.2324(4) 0.7449(5) 0.070(2) Uani 1 1 d .
H66 H -0.3448 0.2258 0.7045 0.084 Uiso 1 1 calc R
Cl1 Cl 0.92269(13) 0.41615(8) 0.89612(8) 0.0537(5) Uani 1 1 d D
Cl2 Cl 0.8932(2) 0.84560(11) 0.90297(10) 0.0841(8) Uani 1 1 d D
O102 O 0.3541(10) 0.1400(5) 0.5906(6) 0.168(5) Uani 1 1 d U
N101 N 0.4300(11) 0.1688(6) 0.6015(7) 0.135(4) Uani 1 1 d U
C103 C 0.4885(13) 0.1781(10) 0.6460(8) 0.173(9) Uani 1 1 d U
O104 O 0.4254(18) 0.2053(6) 0.5433(7) 0.269(11) Uani 1 1 d U
O21 O 0.9859(10) 0.8536(6) 0.9381(8) 0.288(12) Uani 1 1 d DU
O22 O 0.8622(9) 0.7954(4) 0.9228(7) 0.198(6) Uani 1 1 d DU
O23 O 0.8384(13) 0.8893(5) 0.9181(7) 0.278(11) Uani 1 1 d DU
O24 O 0.9079(17) 0.8461(6) 0.8499(6) 0.333(14) Uani 1 1 d DU
O11 O 1.0191(6) 0.3953(4) 0.8973(4) 0.137(4) Uani 1 1 d DU
O12 O 0.9245(11) 0.4702(4) 0.8958(7) 0.251(9) Uani 1 1 d DU
O13 O 0.8736(12) 0.3929(5) 0.8451(7) 0.315(14) Uani 1 1 d DU
O14 O 0.8894(14) 0.3917(8) 0.9397(7) 0.402(18) Uani 1 1 d DU
N201 N 0.728(2) 1.0169(10) 0.9717(13) 0.256(11) Uani 1 1 d U
O204 O 0.863(2) 1.0070(7) 0.9843(9) 0.274(12) Uani 1 1 d U
O202 O 0.8136(10) 1.0226(7) 0.9128(7) 0.191(5) Uani 1 1 d U
C203 C 0.8124(18) 1.030(3) 1.0209(14) 0.40(3) Uani 1 1 d U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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 Co1 N41 95.4(2) . .
N21 Co1 N51 86.9(2) . 2_556
N41 Co1 N51 175.1(2) . 2_556
N21 Co1 N31 172.7(2) . .
N41 Co1 N31 77.3(2) . .
N51 Co1 N31 100.40(18) 2_556 .
N21 Co1 N11 77.7(2) . .
N41 Co1 N11 85.0(2) . .
N51 Co1 N11 99.74(18) 2_556 .
N31 Co1 N11 100.6(2) . .
N21 Co1 N61 98.4(2) . 2_556
N41 Co1 N61 98.5(3) . 2_556
N51 Co1 N61 76.9(2) 2_556 2_556
N31 Co1 N61 83.6(2) . 2_556
N11 Co1 N61 175.1(2) . 2_556
C15 S14 C13 90.7(3) . .
C34 S33 C32 89.3(3) . .
C52 S53 C54 89.6(3) . .
C15 N11 C12 110.7(5) . .
C15 N11 Co1 111.8(5) . .
C12 N11 Co1 136.5(4) . .
C26 N21 C22 117.9(6) . .
C26 N21 Co1 126.1(5) . .
C22 N21 Co1 115.6(5) . .
C32 N31 C35 109.8(5) . .
C32 N31 Co1 112.0(4) . .
C35 N31 Co1 136.4(4) . .
C42 N41 C46 118.4(7) . .
C42 N41 Co1 115.9(5) . .
C46 N41 Co1 124.9(5) . .
C52 N51 C55 110.3(5) . .
C52 N51 Co1 112.5(4) . 2_556
C55 N51 Co1 136.3(4) . 2_556
C62 N61 C66 118.5(7) . .
C62 N61 Co1 114.5(4) . 2_556
C66 N61 Co1 126.0(6) . 2_556
C13 C12 N11 115.5(6) . .
C13 C12 C55 122.4(6) . .
N11 C12 C55 121.9(5) . .
C12 C13 S14 108.7(6) . .
N11 C15 C22 120.5(6) . .
N11 C15 S14 114.3(5) . .
C22 C15 S14 125.1(5) . .
N21 C22 C23 123.3(7) . .
N21 C22 C15 113.6(5) . .
C23 C22 C15 123.1(7) . .
C22 C23 C24 118.1(8) . .
C25 C24 C23 118.0(7) . .
C24 C25 C26 121.0(8) . .
N21 C26 C25 121.4(8) . .
N31 C32 C42 120.1(6) . .
N31 C32 S33 115.4(5) . .
C42 C32 S33 124.4(5) . .
C35 C34 S33 111.0(5) . .
C34 C35 N31 114.5(6) . .
C34 C35 C35 123.0(5) . 2_556
N31 C35 C35 122.4(5) . 2_556
N41 C42 C43 124.5(7) . .
N41 C42 C32 113.2(6) . .
C43 C42 C32 122.2(7) . .
C42 C43 C44 117.6(9) . .
C45 C44 C43 118.9(9) . .
C44 C45 C46 119.8(8) . .
N41 C46 C45 120.8(8) . .
N51 C52 C62 120.7(6) . .
N51 C52 S53 115.4(5) . .
C62 C52 S53 123.8(5) . .
C55 C54 S53 110.0(5) . .
C54 C55 N51 114.6(6) . .
C54 C55 C12 122.9(6) . .
N51 C55 C12 122.5(5) . .
N61 C62 C63 121.8(7) . .
N61 C62 C52 114.6(6) . .
C63 C62 C52 123.6(8) . .
C62 C63 C64 120.9(10) . .
C63 C64 C65 116.6(9) . .
C66 C65 C64 121.2(8) . .
N61 C66 C65 120.8(10) . .
O12 Cl1 O14 117.3(10) . .
O12 Cl1 O13 114.0(9) . .
O14 Cl1 O13 107.4(9) . .
O12 Cl1 O11 109.6(8) . .
O14 Cl1 O11 106.0(9) . .
O13 Cl1 O11 101.2(7) . .
O24 Cl2 O23 115.0(8) . .
O24 Cl2 O22 115.9(8) . .
O23 Cl2 O22 111.5(8) . .
O24 Cl2 O21 106.3(10) . .
O23 Cl2 O21 103.3(9) . .
O22 Cl2 O21 103.1(8) . .
C103 N101 O102 133(2) . .
C103 N101 O104 122.8(18) . .
O102 N101 O104 102.7(16) . .
C203 N201 O204 44.6(15) . .
C203 O204 O202 112(3) . .
C203 O204 N201 54.3(16) . .
O202 O204 N201 66.3(17) . .
O204 C203 N201 81(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N21 2.130(5) .
Co1 N41 2.138(6) .
Co1 N51 2.143(5) 2_556
Co1 N31 2.150(5) .
Co1 N11 2.161(5) .
Co1 N61 2.182(6) 2_556
S14 C15 1.696(7) .
S14 C13 1.730(7) .
S33 C34 1.705(7) .
S33 C32 1.710(7) .
S53 C52 1.698(7) .
S53 C54 1.733(7) .
N11 C15 1.328(7) .
N11 C12 1.377(9) .
N21 C26 1.328(10) .
N21 C22 1.351(9) .
N31 C32 1.318(8) .
N31 C35 1.389(7) .
N41 C42 1.321(9) .
N41 C46 1.349(9) .
N51 C52 1.323(8) .
N51 C55 1.392(7) .
N51 Co1 2.143(5) 2_556
N61 C62 1.320(10) .
N61 C66 1.352(9) .
N61 Co1 2.182(6) 2_556
C12 C13 1.369(9) .
C12 C55 1.459(8) .
C15 C22 1.467(10) .
C22 C23 1.366(9) .
C23 C24 1.407(12) .
C24 C25 1.346(13) .
C25 C26 1.385(11) .
C32 C42 1.478(9) .
C34 C35 1.361(9) .
C35 C35 1.455(12) 2_556
C42 C43 1.364(11) .
C43 C44 1.401(12) .
C44 C45 1.367(16) .
C45 C46 1.395(13) .
C52 C62 1.456(9) .
C54 C55 1.362(9) .
C62 C63 1.358(10) .
C63 C64 1.378(13) .
C64 C65 1.356(15) .
C65 C66 1.368(14) .
Cl1 O12 1.250(9) .
Cl1 O14 1.273(10) .
Cl1 O13 1.331(10) .
Cl1 O11 1.362(7) .
Cl2 O24 1.240(11) .
Cl2 O23 1.322(9) .
Cl2 O22 1.334(8) .
Cl2 O21 1.354(10) .
O102 N101 1.197(15) .
N101 C103 1.173(18) .
N101 O104 1.547(19) .
N201 C203 1.46(3) .
N201 O204 1.77(3) .
O204 C203 1.26(3) .
O204 O202 1.66(3) .
