#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/36/7053690.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7053690
loop_
_publ_author_name
'Wang, Qiang'
'Day, Peter'
'Griffiths, Jon-Paul'
'Nie, Hui'
'Wallis, John D.'
_publ_section_title
;
 Synthetic strategies for preparing BEDT-TTF derivatives functionalised
 with metal ion binding groups
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1790
_journal_paper_doi               10.1039/b606715h
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C20.5 H18 Cl N O2 S9'
_chemical_formula_weight         634.35
_chemical_melting_point          454.5(15)
_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                90.439(1)
_cell_angle_beta                 92.745(1)
_cell_angle_gamma                101.822(1)
_cell_formula_units_Z            2
_cell_length_a                   7.8542(1)
_cell_length_b                   11.9820(2)
_cell_length_c                   14.1992(3)
_cell_measurement_reflns_used    5966
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1306.22(4)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31614
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0377
_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)+(0.0306P)²+2.2279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                5172
_reflns_number_total             5986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606715hsup1.cif
_cod_data_source_block           c:\2005qw~1\qwe228
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '453-456' was changed to '454.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C20.50 H18 Cl N O2 S9'
_cod_database_code               7053690
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
Cl1 Cl 0.00617(15) -0.37243(12) 1.00614(7) 0.0757(3) Uani 1 1 d .
S1 S 0.24710(8) 0.47814(5) 0.48052(4) 0.01995(13) Uani 1 1 d .
S2 S 0.21450(8) 0.58888(5) 0.69954(4) 0.02036(13) Uani 1 1 d .
S3 S 0.21343(7) 0.25587(5) 0.57651(4) 0.01723(12) Uani 1 1 d .
S4 S 0.15715(8) 0.34678(5) 0.76335(4) 0.02202(13) Uani 1 1 d .
S5 S 0.04104(8) 0.00285(5) 0.63755(4) 0.01991(13) Uani 1 1 d .
S6 S -0.02668(8) 0.08849(5) 0.82538(4) 0.02154(13) Uani 1 1 d .
S7 S -0.14625(8) -0.23249(5) 0.66498(4) 0.02246(13) Uani 1 1 d .
S8 S -0.22217(8) -0.13158(5) 0.88984(4) 0.02481(14) Uani 1 1 d .
S9 S 0.30781(8) 0.84936(5) 0.47262(4) 0.02184(13) Uani 1 1 d .
O1 O 0.3461(3) 0.56731(15) 0.17547(14) 0.0380(5) Uani 1 1 d .
O2 O 0.6479(3) 1.15317(14) 0.24640(13) 0.0311(4) Uani 1 1 d .
N1 N 0.5126(2) 0.86402(16) 0.17571(13) 0.0186(4) Uani 1 1 d .
C1 C 0.3364(3) 0.62676(19) 0.51819(16) 0.0182(4) Uani 1 1 d .
H1 H 0.4431 0.6538 0.4823 0.022 Uiso 1 1 calc R
C2 C 0.3914(3) 0.6402(2) 0.62224(16) 0.0200(5) Uani 1 1 d .
H2B H 0.4393 0.7218 0.6369 0.024 Uiso 1 1 calc R
H2A H 0.4856 0.5980 0.6355 0.024 Uiso 1 1 calc R
C3 C 0.2131(3) 0.40306(18) 0.58501(16) 0.0165(4) Uani 1 1 d .
C4 C 0.1902(3) 0.44454(18) 0.67072(16) 0.0174(4) Uani 1 1 d .
C5 C 0.1259(3) 0.22699(19) 0.68746(16) 0.0185(4) Uani 1 1 d .
C6 C 0.0518(3) 0.12100(19) 0.71282(15) 0.0176(4) Uani 1 1 d .
C7 C -0.0861(3) -0.09335(19) 0.71125(15) 0.0171(4) Uani 1 1 d .
C8 C -0.1163(3) -0.05608(19) 0.79710(16) 0.0178(4) Uani 1 1 d .
C9 C -0.1640(3) -0.3089(2) 0.77407(17) 0.0229(5) Uani 1 1 d .
H9A H -0.1996 -0.3917 0.7599 0.028 Uiso 1 1 calc R
H9B H -0.0483 -0.2953 0.8080 0.028 Uiso 1 1 calc R
C10 C -0.2948(3) -0.2733(2) 0.83752(17) 0.0237(5) Uani 1 1 d .
H10A H -0.3190 -0.3291 0.8887 0.028 Uiso 1 1 calc R
H10B H -0.4053 -0.2757 0.8002 0.028 Uiso 1 1 calc R
C11 C 0.2056(3) 0.70135(19) 0.48946(17) 0.0202(5) Uani 1 1 d .
H11B H 0.1198 0.6974 0.5388 0.024 Uiso 1 1 calc R
H11A H 0.1415 0.6702 0.4301 0.024 Uiso 1 1 calc R
C22 C 0.4308(3) 0.76442(19) 0.21009(16) 0.0188(5) Uani 1 1 d .
C23 C 0.3634(3) 0.75200(19) 0.29920(16) 0.0190(5) Uani 1 1 d .
H23 H 0.3065 0.6792 0.3198 0.023 Uiso 1 1 calc R
C24 C 0.3807(3) 0.84816(19) 0.35780(15) 0.0178(4) Uani 1 1 d .
C25 C 0.4653(3) 0.95280(19) 0.32239(16) 0.0191(5) Uani 1 1 d .
H25 H 0.4795 1.0207 0.3595 0.023 Uiso 1 1 calc R
C26 C 0.5282(3) 0.95609(19) 0.23264(16) 0.0185(4) Uani 1 1 d .
C27 C 0.4164(3) 0.6603(2) 0.14801(17) 0.0246(5) Uani 1 1 d .
C28 C 0.4908(4) 0.6762(2) 0.05263(18) 0.0287(6) Uani 1 1 d .
H28C H 0.4806 0.6017 0.0215 0.043 Uiso 1 1 calc R
H28B H 0.6139 0.7141 0.0596 0.043 Uiso 1 1 calc R
H28A H 0.4267 0.7232 0.0144 0.043 Uiso 1 1 calc R
C29 C 0.6232(3) 1.06858(19) 0.19571(17) 0.0206(5) Uani 1 1 d .
C30 C 0.6855(3) 1.0718(2) 0.09738(17) 0.0238(5) Uani 1 1 d .
H30C H 0.5861 1.0668 0.0520 0.036 Uiso 1 1 calc R
H30A H 0.7422 1.0074 0.0871 0.036 Uiso 1 1 calc R
H30B H 0.7690 1.1435 0.0888 0.036 Uiso 1 1 calc R
C40 C -0.0430(9) -0.5129(9) 1.0548(4) 0.070(3) Uani 0.50 1 d P
H40A H 0.0234 -0.5095 1.1161 0.084 Uiso 0.50 1 calc PR
H40B H -0.1680 -0.5290 1.0685 0.084 Uiso 0.50 1 calc PR
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
C40 Cl1 C40 59.2(3) 2_547
C3 S1 C1 104.96(10) .
C4 S2 C2 96.47(11) .
C5 S3 C3 93.45(10) .
C5 S4 C4 93.70(11) .
C7 S5 C6 94.55(10) .
C6 S6 C8 94.69(10) .
C7 S7 C9 98.83(11) .
C8 S8 C10 101.90(11) .
C24 S9 C11 102.88(11) .
C22 N1 C26 116.33(19) .
C2 C1 C11 112.08(19) .
C2 C1 S1 113.59(16) .
C11 C1 S1 109.43(15) .
C1 C2 S2 113.54(16) .
C4 C3 S1 127.62(17) .
C4 C3 S3 116.85(17) .
S1 C3 S3 115.52(12) .
C3 C4 S2 124.91(18) .
C3 C4 S4 117.15(17) .
S2 C4 S4 117.54(13) .
C6 C5 S4 123.71(18) .
C6 C5 S3 122.21(17) .
S4 C5 S3 113.96(13) .
C5 C6 S5 121.68(17) .
C5 C6 S6 123.20(17) .
S5 C6 S6 114.97(13) .
C8 C7 S7 127.55(18) .
C8 C7 S5 118.16(17) .
S7 C7 S5 114.12(12) .
C7 C8 S8 129.61(18) .
C7 C8 S6 116.58(17) .
S8 C8 S6 113.69(12) .
C10 C9 S7 112.54(17) .
C9 C10 S8 113.75(17) .
C1 C11 S9 113.14(16) .
N1 C22 C23 124.2(2) .
N1 C22 C27 116.8(2) .
C23 C22 C27 118.9(2) .
C22 C23 C24 119.0(2) .
C23 C24 C25 117.3(2) .
C23 C24 S9 125.66(18) .
C25 C24 S9 117.03(17) .
C26 C25 C24 119.3(2) .
N1 C26 C25 123.9(2) .
N1 C26 C29 117.0(2) .
C25 C26 C29 119.1(2) .
O1 C27 C28 122.1(2) .
O1 C27 C22 120.1(2) .
C28 C27 C22 117.8(2) .
O2 C29 C30 122.0(2) .
O2 C29 C26 119.3(2) .
C30 C29 C26 118.6(2) .
Cl1 C40 Cl1 120.8(3) 2_547
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 C40 1.699(9) 2_547
Cl1 C40 1.799(10) .
S1 C3 1.744(2) .
S1 C1 1.840(2) .
S2 C4 1.744(2) .
S2 C2 1.822(2) .
S3 C5 1.758(2) .
S3 C3 1.767(2) .
S4 C5 1.757(2) .
S4 C4 1.761(2) .
S5 C7 1.752(2) .
S5 C6 1.753(2) .
S6 C6 1.758(2) .
S6 C8 1.766(2) .
S7 C7 1.751(2) .
S7 C9 1.802(2) .
S8 C8 1.749(2) .
S8 C10 1.817(2) .
S9 C24 1.755(2) .
S9 C11 1.813(2) .
O1 C27 1.214(3) .
O2 C29 1.216(3) .
N1 C22 1.342(3) .
N1 C26 1.344(3) .
C1 C2 1.517(3) .
C1 C11 1.537(3) .
C3 C4 1.345(3) .
C5 C6 1.344(3) .
C7 C8 1.343(3) .
C9 C10 1.521(3) .
C22 C23 1.392(3) .
C22 C27 1.504(3) .
C23 C24 1.396(3) .
C24 C25 1.402(3) .
C25 C26 1.386(3) .
C26 C29 1.512(3) .
C27 C28 1.499(3) .
C29 C30 1.500(3) .
C40 Cl1 1.699(9) 2_547
