#------------------------------------------------------------------------------
#$Date: 2016-02-14 05:40:26 +0100 (Sun 14 de Feb de 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/89/7208918.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_7208918
loop_
_publ_author_name
'Shao, Ming-Yan'
'Huo, Peng'
'Sun, Yong-Gang'
'Li, Xin-Yu'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 Synthetic methods and structural study of coordination polymers of Cd(ii)
 and Co(ii) with tetrathiafulvalene--tetracarboxylate
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1086
_journal_paper_doi               10.1039/c2ce26219c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C18 H20 Co N2 O9 S2'
_chemical_formula_weight         531.41
_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                106.620(2)
_cell_angle_beta                 103.906(3)
_cell_angle_gamma                102.182(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0480(11)
_cell_length_b                   10.9486(15)
_cell_length_c                   12.7222(18)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1118.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9088
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.7522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.694
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0018P)²+15.4884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                3060
_reflns_number_total             3820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26219c.txt
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7208918
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
Co1 Co 0.59905(13) -0.01902(11) 0.38176(9) 0.0398(3) Uani 1 1 d .
S1 S 0.98202(18) 0.30188(15) 0.88156(13) 0.0213(4) Uani 1 1 d .
S2 S 0.80369(18) 0.49455(15) 0.85797(13) 0.0215(4) Uani 1 1 d .
N1 N 0.4309(6) 0.0753(5) 0.2531(4) 0.0191(11) Uani 1 1 d .
N2 N 0.5194(6) -0.1455(5) 0.1648(4) 0.0205(11) Uani 1 1 d .
C1 C 0.8158(6) 0.2501(5) 0.7558(4) 0.0131(11) Uani 1 1 d .
C2 C 0.7355(6) 0.3390(5) 0.7457(4) 0.0112(11) Uani 1 1 d .
C3 C 0.9548(7) 0.4569(6) 0.9462(5) 0.0160(12) Uani 1 1 d .
C4 C 0.7919(7) 0.1143(5) 0.6719(5) 0.0131(11) Uani 1 1 d .
C5 C 0.5932(7) 0.3313(6) 0.6498(5) 0.0154(12) Uani 1 1 d .
C6 C 0.3870(8) 0.1823(6) 0.2944(6) 0.0252(14) Uani 1 1 d .
H6 H 0.4299 0.2312 0.3744 0.030 Uiso 1 1 calc R
C7 C 0.2807(8) 0.2272(7) 0.2264(6) 0.0300(15) Uani 1 1 d .
H7 H 0.2546 0.3048 0.2598 0.036 Uiso 1 1 calc R
C8 C 0.2157(8) 0.1553(7) 0.1099(6) 0.0263(15) Uani 1 1 d .
H8 H 0.1419 0.1819 0.0625 0.032 Uiso 1 1 calc R
C9 C 0.2592(7) 0.0432(6) 0.0624(5) 0.0228(14) Uani 1 1 d .
C10 C 0.3664(7) 0.0039(6) 0.1360(5) 0.0160(12) Uani 1 1 d .
C11 C 0.5683(8) -0.2486(7) 0.1221(6) 0.0269(15) Uani 1 1 d .
H11 H 0.6401 -0.2727 0.1733 0.032 Uiso 1 1 calc R
C12 C 0.5172(9) -0.3238(7) 0.0031(6) 0.0318(16) Uani 1 1 d .
H12 H 0.5551 -0.3963 -0.0242 0.038 Uiso 1 1 calc R
C13 C 0.4134(9) -0.2914(7) -0.0717(6) 0.0332(17) Uani 1 1 d .
H13 H 0.3791 -0.3410 -0.1515 0.040 Uiso 1 1 calc R
C14 C 0.3567(8) -0.1830(7) -0.0302(5) 0.0249(14) Uani 1 1 d .
C15 C 0.4172(7) -0.1101(6) 0.0917(5) 0.0176(12) Uani 1 1 d .
C16 C 0.2001(8) -0.0347(7) -0.0602(5) 0.0279(15) Uani 1 1 d .
H16 H 0.1274 -0.0103 -0.1107 0.034 Uiso 1 1 calc R
C17 C 0.2472(9) -0.1404(8) -0.1026(6) 0.0345(17) Uani 1 1 d .
H17 H 0.2072 -0.1886 -0.1828 0.041 Uiso 1 1 calc R
C18 C 0.9429(11) 0.4838(10) 0.3365(8) 0.056(2) Uani 1 1 d .
H18A H 1.0044 0.5569 0.4089 0.084 Uiso 1 1 calc R
H18B H 0.9105 0.5195 0.2761 0.084 Uiso 1 1 calc R
H18C H 1.0079 0.4269 0.3154 0.084 Uiso 1 1 calc R
O1 O 0.9016(5) 0.0641(4) 0.6953(4) 0.0218(9) Uani 1 1 d .
O2 O 0.6643(5) 0.0589(4) 0.5870(3) 0.0176(9) Uani 1 1 d .
O3 O 0.4750(5) 0.2304(4) 0.6060(4) 0.0249(10) Uani 1 1 d .
O4 O 0.6025(5) 0.4352(4) 0.6265(4) 0.0315(12) Uani 1 1 d .
O5 O 0.8257(5) -0.0940(5) 0.3795(4) 0.0297(11) Uani 1 1 d .
O6 O 0.7889(5) 0.1828(4) 0.4113(4) 0.0276(10) Uani 1 1 d .
O7 O 0.8066(6) 0.4087(5) 0.3499(4) 0.0351(12) Uani 1 1 d .
H7A H 0.7626 0.4600 0.3828 0.053 Uiso 1 1 calc R
O8 O 0.6911(5) 0.5690(4) 0.4917(4) 0.0251(10) Uani 1 1 d .
O9 O 0.0971(5) 0.1830(4) 0.4392(4) 0.0263(10) 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'
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'
Co Co 0.3494 0.9721 '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
O3 Co1 O6 152.99(15) 2_656 .
O3 Co1 O5 75.92(16) 2_656 .
O6 Co1 O5 79.99(16) . .
O3 Co1 O2 84.47(15) 2_656 .
O6 Co1 O2 85.68(16) . .
O5 Co1 O2 95.06(16) . .
C1 S1 C3 95.3(3) . .
C2 S2 C3 95.5(3) . .
C6 N1 C10 117.4(5) . .
C11 N2 C15 119.0(5) . .
C2 C1 C4 129.6(5) . .
C2 C1 S1 116.7(4) . .
C4 C1 S1 113.6(4) . .
C1 C2 C5 131.2(5) . .
C1 C2 S2 117.6(4) . .
C5 C2 S2 111.2(4) . .
C3 C3 S2 121.9(6) 2_767 .
C3 C3 S1 123.5(6) 2_767 .
S2 C3 S1 114.5(3) . .
O1 C4 O2 125.7(5) . .
O1 C4 C1 115.4(5) . .
O2 C4 C1 119.0(5) . .
O3 C5 O4 124.8(5) . .
O3 C5 C2 120.3(5) . .
O4 C5 C2 114.7(5) . .
N1 C6 C7 124.1(6) . .
N1 C6 H6 118.0 . .
C7 C6 H6 118.0 . .
C8 C7 C6 118.3(6) . .
C8 C7 H7 120.8 . .
C6 C7 H7 120.8 . .
C7 C8 C9 119.7(6) . .
C7 C8 H8 120.1 . .
C9 C8 H8 120.1 . .
C8 C9 C10 118.7(6) . .
C8 C9 C16 122.8(6) . .
C10 C9 C16 118.5(6) . .
N1 C10 C9 121.7(6) . .
N1 C10 C15 117.0(5) . .
C9 C10 C15 121.3(5) . .
N2 C11 C12 122.5(6) . .
N2 C11 H11 118.7 . .
C12 C11 H11 118.7 . .
C13 C12 C11 119.7(6) . .
C13 C12 H12 120.2 . .
C11 C12 H12 120.2 . .
C12 C13 C14 119.8(6) . .
C12 C13 H13 120.1 . .
C14 C13 H13 120.1 . .
C13 C14 C15 116.9(6) . .
C13 C14 C17 124.0(6) . .
C15 C14 C17 119.0(6) . .
N2 C15 C14 122.0(6) . .
N2 C15 C10 119.8(5) . .
C14 C15 C10 118.2(5) . .
C17 C16 C9 120.9(6) . .
C17 C16 H16 119.6 . .
C9 C16 H16 119.6 . .
C16 C17 C14 122.2(6) . .
C16 C17 H17 118.9 . .
C14 C17 H17 118.9 . .
O7 C18 H18A 109.5 . .
O7 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O7 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C4 O2 Co1 135.4(4) . .
C5 O3 Co1 137.7(4) . 2_656
C18 O7 H7A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.331(4) 2_656
Co1 O6 2.363(4) .
Co1 O5 2.368(5) .
Co1 O2 2.380(4) .
S1 C1 1.763(5) .
S1 C3 1.759(6) .
S2 C2 1.750(5) .
S2 C3 1.750(6) .
N1 C6 1.324(8) .
N1 C10 1.376(8) .
N2 C11 1.319(8) .
N2 C15 1.346(8) .
C1 C2 1.349(8) .
C1 C4 1.497(8) .
C2 C5 1.514(7) .
C3 C3 1.354(11) 2_767
C4 O1 1.248(7) .
C4 O2 1.265(7) .
C5 O3 1.240(7) .
C5 O4 1.246(7) .
C6 C7 1.399(9) .
C6 H6 0.9400 .
C7 C8 1.371(10) .
C7 H7 0.9400 .
C8 C9 1.387(10) .
C8 H8 0.9400 .
C9 C10 1.404(9) .
C9 C16 1.446(9) .
C10 C15 1.433(9) .
C11 C12 1.404(10) .
C11 H11 0.9400 .
C12 C13 1.348(11) .
C12 H12 0.9400 .
C13 C14 1.407(10) .
C13 H13 0.9400 .
C14 C15 1.428(8) .
C14 C17 1.433(10) .
C16 C17 1.332(10) .
C16 H16 0.9400 .
C17 H17 0.9400 .
C18 O7 1.407(10) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
O3 Co1 2.331(4) 2_656
O7 H7A 0.8300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C3 S1 C1 C2 4.1(5) . .
C3 S1 C1 C4 -179.6(4) . .
C4 C1 C2 C5 2.2(10) . .
S1 C1 C2 C5 177.7(5) . .
C4 C1 C2 S2 -176.0(5) . .
S1 C1 C2 S2 -0.4(6) . .
C3 S2 C2 C1 -3.5(5) . .
C3 S2 C2 C5 177.9(4) . .
C2 S2 C3 C3 -175.6(7) . 2_767
C2 S2 C3 S1 6.3(4) . .
C1 S1 C3 C3 175.5(8) . 2_767
C1 S1 C3 S2 -6.4(4) . .
C2 C1 C4 O1 167.5(6) . .
S1 C1 C4 O1 -8.2(6) . .
C2 C1 C4 O2 -14.4(9) . .
S1 C1 C4 O2 170.0(4) . .
C1 C2 C5 O3 46.5(9) . .
S2 C2 C5 O3 -135.3(5) . .
C1 C2 C5 O4 -138.1(7) . .
S2 C2 C5 O4 40.2(6) . .
C10 N1 C6 C7 -0.5(10) . .
N1 C6 C7 C8 1.0(11) . .
C6 C7 C8 C9 -1.6(10) . .
C7 C8 C9 C10 1.7(9) . .
C7 C8 C9 C16 -177.7(6) . .
C6 N1 C10 C9 0.6(8) . .
C6 N1 C10 C15 178.7(5) . .
C8 C9 C10 N1 -1.2(9) . .
C16 C9 C10 N1 178.2(6) . .
C8 C9 C10 C15 -179.2(6) . .
C16 C9 C10 C15 0.2(9) . .
C15 N2 C11 C12 -0.4(10) . .
N2 C11 C12 C13 -0.4(11) . .
C11 C12 C13 C14 -0.3(11) . .
C12 C13 C14 C15 1.6(10) . .
C12 C13 C14 C17 179.7(7) . .
C11 N2 C15 C14 1.8(9) . .
C11 N2 C15 C10 -178.2(6) . .
C13 C14 C15 N2 -2.4(9) . .
C17 C14 C15 N2 179.4(6) . .
C13 C14 C15 C10 177.6(6) . .
C17 C14 C15 C10 -0.6(9) . .
N1 C10 C15 N2 2.3(8) . .
C9 C10 C15 N2 -179.6(5) . .
N1 C10 C15 C14 -177.7(5) . .
C9 C10 C15 C14 0.4(9) . .
C8 C9 C16 C17 178.8(7) . .
C10 C9 C16 C17 -0.6(10) . .
C9 C16 C17 C14 0.4(11) . .
C13 C14 C17 C16 -177.9(7) . .
C15 C14 C17 C16 0.2(11) . .
O1 C4 O2 Co1 -62.8(8) . .
C1 C4 O2 Co1 119.3(5) . .
O3 Co1 O2 C4 111.1(5) 2_656 .
O6 Co1 O2 C4 -43.8(5) . .
O5 Co1 O2 C4 35.8(5) . .
O4 C5 O3 Co1 179.4(5) . 2_656
C2 C5 O3 Co1 -5.6(9) . 2_656
