#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:16:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180069 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/15/7051565.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_7051565
loop_
_publ_author_name
'Constable, Edwin C.'
'Hermann, B. A.'
'Housecroft, Catherine E.'
'Neuburger, Markus'
'Schaffner, Silvia'
'Scherer, Lukas J.'
_publ_section_title
;
 2,2′:6′,2″-Terpyridine-4′(1′H)-thione:
 a missing link in metallosupramolecular chemistry
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1475
_journal_paper_doi               10.1039/b510792j
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C30 H20 N6 S2'
_chemical_formula_sum            'C30 H20 N6 S2'
_chemical_formula_weight         528.66
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-08-24
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 120.5668(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5557(4)
_cell_length_b                   5.5221(2)
_cell_length_c                   22.6510(9)
_cell_measurement_reflns_used    5906
_cell_measurement_temperature    173
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     1244.54(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12042
_diffrn_reflns_theta_full        28.544
_diffrn_reflns_theta_max         29.127
_diffrn_reflns_theta_min         3.526
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1876
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000146
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.574 0.621 0.353
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0746
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0465
_reflns_limit_h_max              13
_reflns_limit_h_min              -15
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                1876
_reflns_number_total             3333
_reflns_threshold_expression     I>1.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2293(6)
_oxford_structure_analysis_title '8241153 ls_a95_173k'
_cod_data_source_file            b510792j.txt
_cod_data_source_block           ls_a95_173k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7051565
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y,-z+1/2
x,-y,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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
S1 S 0.47844(6) 0.41909(11) 0.20065(3) 0.0389 1.0000 Uani . . . . . .
N1 N 0.6463(2) 0.2195(4) 0.02955(10) 0.0500 1.0000 Uani . . . . . .
N2 N 0.75318(17) -0.1307(3) 0.18267(9) 0.0336 1.0000 Uani . . . . . .
N3 N 0.8241(2) -0.2982(4) 0.35135(10) 0.0423 1.0000 Uani . . . . . .
C1 C 0.6594(3) 0.2187(6) -0.02610(13) 0.0568 1.0000 Uani . . . . . .
C2 C 0.7232(2) 0.0428(6) -0.04115(12) 0.0495 1.0000 Uani . . . . . .
C3 C 0.7778(3) -0.1480(6) 0.00404(14) 0.0565 1.0000 Uani . . . . . .
C4 C 0.7661(3) -0.1543(5) 0.06190(13) 0.0480 1.0000 Uani . . . . . .
C5 C 0.6996(2) 0.0326(4) 0.07284(11) 0.0359 1.0000 Uani . . . . . .
C6 C 0.6842(2) 0.0374(4) 0.13430(11) 0.0331 1.0000 Uani . . . . . .
C7 C 0.6017(2) 0.2082(4) 0.13982(11) 0.0357 1.0000 Uani . . . . . .
C8 C 0.58806(19) 0.2016(4) 0.19738(11) 0.0327 1.0000 Uani . . . . . .
C9 C 0.65733(19) 0.0266(4) 0.24763(11) 0.0331 1.0000 Uani . . . . . .
C10 C 0.7401(2) -0.1325(4) 0.23823(11) 0.0324 1.0000 Uani . . . . . .
C11 C 0.82028(19) -0.3191(4) 0.29120(10) 0.0332 1.0000 Uani . . . . . .
C12 C 0.8863(2) -0.5031(5) 0.27803(12) 0.0387 1.0000 Uani . . . . . .
C13 C 0.9587(2) -0.6732(5) 0.32862(13) 0.0450 1.0000 Uani . . . . . .
C14 C 0.9626(2) -0.6534(5) 0.39034(13) 0.0490 1.0000 Uani . . . . . .
C15 C 0.8945(2) -0.4655(5) 0.39911(13) 0.0507 1.0000 Uani . . . . . .
H11 H 0.6196 0.3573 -0.0588 0.0680 1.0000 Uiso R . . . . .
H21 H 0.7300 0.0517 -0.0834 0.0593 1.0000 Uiso R . . . . .
H31 H 0.8255 -0.2810 -0.0049 0.0724 1.0000 Uiso R . . . . .
H41 H 0.8050 -0.2916 0.0952 0.0606 1.0000 Uiso R . . . . .
H71 H 0.5534 0.3328 0.1033 0.0424 1.0000 Uiso R . . . . .
H91 H 0.6479 0.0156 0.2891 0.0415 1.0000 Uiso R . . . . .
H121 H 0.8817 -0.5124 0.2328 0.0444 1.0000 Uiso R . . . . .
H131 H 1.0070 -0.8076 0.3206 0.0502 1.0000 Uiso R . . . . .
H141 H 1.0140 -0.7731 0.4279 0.0532 1.0000 Uiso R . . . . .
H151 H 0.8979 -0.4533 0.4440 0.0606 1.0000 Uiso R . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 3_655 S1 . C8 . 105.41(8) yes
C1 . N1 . C5 . 117.1(2) yes
C6 . N2 . C10 . 117.81(18) yes
C11 . N3 . C15 . 116.9(2) yes
N1 . C1 . C2 . 124.8(3) yes
N1 . C1 . H11 . 117.618 no
C2 . C1 . H11 . 117.629 no
C1 . C2 . C3 . 117.4(2) yes
C1 . C2 . H21 . 121.294 no
C3 . C2 . H21 . 121.290 no
C2 . C3 . C4 . 119.6(3) yes
C2 . C3 . H31 . 120.172 no
C4 . C3 . H31 . 120.188 no
C3 . C4 . C5 . 118.8(2) yes
C3 . C4 . H41 . 120.602 no
C5 . C4 . H41 . 120.632 no
C4 . C5 . N1 . 122.4(2) yes
C4 . C5 . C6 . 121.5(2) yes
N1 . C5 . C6 . 116.2(2) yes
C5 . C6 . N2 . 116.46(19) yes
C5 . C6 . C7 . 120.58(19) yes
N2 . C6 . C7 . 123.0(2) yes
C6 . C7 . C8 . 118.4(2) yes
C6 . C7 . H71 . 120.792 no
C8 . C7 . H71 . 120.791 no
S1 . C8 . C7 . 116.43(17) yes
S1 . C8 . C9 . 124.11(16) yes
C7 . C8 . C9 . 119.4(2) yes
C8 . C9 . C10 . 117.8(2) yes
C8 . C9 . H91 . 121.107 no
C10 . C9 . H91 . 121.102 no
C9 . C10 . N2 . 123.5(2) yes
C9 . C10 . C11 . 120.40(19) yes
N2 . C10 . C11 . 116.07(19) yes
C10 . C11 . N3 . 116.2(2) yes
C10 . C11 . C12 . 121.0(2) yes
N3 . C11 . C12 . 122.7(2) yes
C11 . C12 . C13 . 118.9(2) yes
C11 . C12 . H121 . 120.550 no
C13 . C12 . H121 . 120.521 no
C12 . C13 . C14 . 118.7(2) yes
C12 . C13 . H131 . 120.669 no
C14 . C13 . H131 . 120.667 no
C13 . C14 . C15 . 118.6(2) yes
C13 . C14 . H141 . 120.674 no
C15 . C14 . H141 . 120.704 no
C14 . C15 . N3 . 124.1(2) yes
C14 . C15 . H151 . 117.917 no
N3 . C15 . H151 . 117.939 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . S1 3_655 2.0281(12) yes
S1 . C8 . 1.774(2) yes
N1 . C1 . 1.344(3) yes
N1 . C5 . 1.339(3) yes
N2 . C6 . 1.345(3) yes
N2 . C10 . 1.342(3) yes
N3 . C11 . 1.346(3) yes
N3 . C15 . 1.338(3) yes
C1 . C2 . 1.363(4) yes
C1 . H11 . 1.000 no
C2 . C3 . 1.378(4) yes
C2 . H21 . 1.000 no
C3 . C4 . 1.385(3) yes
C3 . H31 . 1.000 no
C4 . C5 . 1.382(3) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.491(3) yes
C6 . C7 . 1.391(3) yes
C7 . C8 . 1.391(3) yes
C7 . H71 . 1.000 no
C8 . C9 . 1.394(3) yes
C9 . C10 . 1.393(3) yes
C9 . H91 . 1.000 no
C10 . C11 . 1.493(3) yes
C11 . C12 . 1.391(3) yes
C12 . C13 . 1.386(3) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.380(4) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.376(4) yes
C14 . H141 . 1.000 no
C15 . H151 . 1.000 no
