#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180118 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/16/7101647.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_7101647
loop_
_publ_author_name
'Gavrilenko, Konstantin S'
'Gal, Yann Le'
'Cador, Olivier'
'Golhen, Stéphane'
'Ouahab, Lahcène'
_publ_section_title
;
 First trinuclear paramagnetic transition metal complexes with redox
 active ligands derived from TTF: Co2M(PhCOO)6(TTF-CH=CH-py)2.2CH3CN, M
 = CoII, MnII.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              280
_journal_page_last               282
_journal_paper_doi               10.1039/b613191c
_journal_year                    2007
_chemical_formula_sum            'C72 H54 Co3 N4 O12 S8'
_chemical_formula_weight         1600.46
_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                94.946(2)
_cell_angle_beta                 105.939(2)
_cell_angle_gamma                90.940(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7106(5)
_cell_length_b                   11.7808(7)
_cell_length_c                   15.0518(11)
_cell_measurement_reflns_used    5210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.998
_cell_volume                     1817.82(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10126
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             819
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.2834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                3440
_reflns_number_total             6173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613191c.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101647
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
C1 C 0.4043(5) 0.2428(5) 0.4589(4) 0.0589(13) Uani 1 1 d .
C2 C 0.4093(5) 0.1368(5) 0.3953(4) 0.0627(14) Uani 1 1 d .
C3 C 0.4611(7) 0.1421(6) 0.3231(5) 0.100(2) Uani 1 1 d .
H3 H 0.4916 0.2120 0.3112 0.120 Uiso 1 1 calc R
C4 C 0.4692(9) 0.0449(8) 0.2669(5) 0.116(3) Uani 1 1 d .
H4 H 0.5072 0.0497 0.2186 0.140 Uiso 1 1 calc R
C5 C 0.4229(7) -0.0565(7) 0.2812(6) 0.102(2) Uani 1 1 d .
H5 H 0.4270 -0.1211 0.2423 0.123 Uiso 1 1 calc R
C6 C 0.3702(8) -0.0642(6) 0.3525(6) 0.109(2) Uani 1 1 d .
H6 H 0.3390 -0.1345 0.3631 0.130 Uiso 1 1 calc R
C7 C 0.3625(6) 0.0333(6) 0.4104(5) 0.0904(19) Uani 1 1 d .
H7 H 0.3257 0.0279 0.4592 0.108 Uiso 1 1 calc R
C8 C 0.2426(5) 0.5426(5) 0.5525(4) 0.0586(13) Uani 1 1 d .
C9 C 0.1532(5) 0.6395(4) 0.5503(4) 0.0588(13) Uani 1 1 d .
C10 C 0.1727(6) 0.7365(6) 0.5103(5) 0.0900(19) Uani 1 1 d .
H10 H 0.2413 0.7422 0.4839 0.108 Uiso 1 1 calc R
C11 C 0.0890(8) 0.8269(6) 0.5094(6) 0.110(3) Uani 1 1 d .
H11 H 0.1018 0.8923 0.4820 0.132 Uiso 1 1 calc R
C12 C -0.0106(8) 0.8194(7) 0.5483(6) 0.103(2) Uani 1 1 d .
H12 H -0.0652 0.8800 0.5478 0.124 Uiso 1 1 calc R
C13 C -0.0311(6) 0.7248(7) 0.5877(5) 0.102(2) Uani 1 1 d .
H13 H -0.0995 0.7205 0.6145 0.123 Uiso 1 1 calc R
C14 C 0.0494(5) 0.6342(5) 0.5885(4) 0.0811(18) Uani 1 1 d .
H14 H 0.0338 0.5688 0.6149 0.097 Uiso 1 1 calc R
C15 C 0.5726(5) 0.4056(4) 0.7069(4) 0.0547(12) Uani 1 1 d .
C16 C 0.7096(5) 0.4325(5) 0.7624(3) 0.0576(13) Uani 1 1 d .
C17 C 0.7867(6) 0.5096(5) 0.7350(4) 0.0787(17) Uani 1 1 d .
H17 H 0.7537 0.5441 0.6806 0.094 Uiso 1 1 calc R
C18 C 0.9121(6) 0.5357(7) 0.7880(5) 0.095(2) Uani 1 1 d .
H18 H 0.9633 0.5890 0.7703 0.114 Uiso 1 1 calc R
C19 C 0.9609(6) 0.4829(7) 0.8666(5) 0.094(2) Uani 1 1 d .
H19 H 1.0465 0.4994 0.9012 0.113 Uiso 1 1 calc R
C20 C 0.8865(6) 0.4060(6) 0.8959(5) 0.0874(19) Uani 1 1 d .
H20 H 0.9213 0.3713 0.9500 0.105 Uiso 1 1 calc R
C21 C 0.7601(6) 0.3808(5) 0.8443(4) 0.0675(15) Uani 1 1 d .
H21 H 0.7084 0.3297 0.8639 0.081 Uiso 1 1 calc R
C22 C 0.1294(6) 0.2834(5) 0.7110(4) 0.0762(17) Uani 1 1 d .
H22 H 0.1172 0.3610 0.7076 0.091 Uiso 1 1 calc R
C23 C 0.0550(6) 0.2233(5) 0.7533(5) 0.0826(18) Uani 1 1 d .
H23 H -0.0052 0.2608 0.7781 0.099 Uiso 1 1 calc R
C24 C 0.0687(5) 0.1075(5) 0.7595(4) 0.0668(14) Uani 1 1 d .
C25 C 0.1582(5) 0.0581(5) 0.7181(4) 0.0702(15) Uani 1 1 d .
H25 H 0.1697 -0.0200 0.7180 0.084 Uiso 1 1 calc R
C26 C 0.2292(5) 0.1234(5) 0.6775(4) 0.0672(15) Uani 1 1 d .
H26 H 0.2883 0.0877 0.6504 0.081 Uiso 1 1 calc R
C27 C -0.0054(5) 0.0400(5) 0.8067(4) 0.0727(16) Uani 1 1 d .
H27 H -0.0076 -0.0391 0.7964 0.087 Uiso 1 1 calc R
C28 C -0.0690(6) 0.0870(5) 0.8634(4) 0.0812(17) Uani 1 1 d .
H28 H -0.0630 0.1661 0.8730 0.097 Uiso 1 1 calc R
C29 C -0.1484(6) 0.0288(6) 0.9130(4) 0.0798(17) Uani 1 1 d .
C30 C -0.2116(6) 0.0864(5) 0.9663(5) 0.0880(19) Uani 1 1 d .
H30 H -0.2031 0.1655 0.9761 0.106 Uiso 1 1 calc R
C31 C -0.2674(5) -0.1224(5) 0.9764(4) 0.0734(16) Uani 1 1 d .
C32 C -0.3093(5) -0.2190(5) 1.0001(4) 0.0687(15) Uani 1 1 d .
C33 C -0.3988(7) -0.3689(6) 1.0788(5) 0.099(2) Uani 1 1 d .
H33 H -0.4367 -0.4062 1.1174 0.119 Uiso 1 1 calc R
C34 C -0.3353(7) -0.4259(6) 1.0271(5) 0.100(2) Uani 1 1 d .
H34 H -0.3290 -0.5045 1.0275 0.120 Uiso 1 1 calc R
C35 C 0.7119(11) 0.3137(10) 0.1540(8) 0.140(4) Uani 1 1 d .
C36 C 0.6193(12) 0.3261(12) 0.2005(7) 0.206(6) Uani 1 1 d .
H36A H 0.6290 0.4009 0.2330 0.309 Uiso 1 1 calc R
H36B H 0.6293 0.2699 0.2442 0.309 Uiso 1 1 calc R
H36C H 0.5346 0.3162 0.1571 0.309 Uiso 1 1 calc R
N1 N 0.2184(4) 0.2356(4) 0.6745(3) 0.0628(11) Uani 1 1 d .
N2 N 0.7847(11) 0.3098(10) 0.1126(9) 0.203(5) Uani 1 1 d .
O1 O 0.4445(4) 0.3351(3) 0.4395(3) 0.0764(11) Uani 1 1 d .
O2 O 0.3585(3) 0.2287(3) 0.5258(3) 0.0693(10) Uani 1 1 d .
O3 O 0.3135(3) 0.5410(3) 0.4999(3) 0.0742(11) Uani 1 1 d .
O4 O 0.2376(3) 0.4686(3) 0.6081(3) 0.0686(10) Uani 1 1 d .
O5 O 0.5295(3) 0.4451(3) 0.6316(2) 0.0678(10) Uani 1 1 d .
O6 O 0.5003(3) 0.3428(3) 0.7379(2) 0.0653(9) Uani 1 1 d .
S1 S -0.16716(16) -0.11826(14) 0.90113(13) 0.0848(5) Uani 1 1 d .
S2 S -0.30936(18) 0.01143(15) 1.01669(14) 0.0952(6) Uani 1 1 d .
S3 S -0.26493(18) -0.35237(15) 0.95922(13) 0.0912(5) Uani 1 1 d .
S4 S -0.41011(16) -0.22654(14) 1.07354(12) 0.0825(5) Uani 1 1 d .
Co1 Co 0.5000 0.5000 0.5000 0.0531(3) Uani 1 2 d S
Co2 Co 0.34087(6) 0.33405(6) 0.62677(5) 0.0582(2) 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
O1 C1 O2 126.4(5) . .
O1 C1 C2 117.4(5) . .
O2 C1 C2 116.2(5) . .
C3 C2 C7 118.6(6) . .
C3 C2 C1 120.8(6) . .
C7 C2 C1 120.6(5) . .
C2 C3 C4 120.8(7) . .
C5 C4 C3 120.7(8) . .
C4 C5 C6 119.8(7) . .
C5 C6 C7 120.1(8) . .
C2 C7 C6 120.0(7) . .
O3 C8 O4 125.9(5) . .
O3 C8 C9 117.6(5) . .
O4 C8 C9 116.5(4) . .
C10 C9 C14 118.3(5) . .
C10 C9 C8 120.4(5) . .
C14 C9 C8 121.3(5) . .
C9 C10 C11 119.8(6) . .
C12 C11 C10 120.3(7) . .
C13 C12 C11 120.6(7) . .
C12 C13 C14 120.0(7) . .
C13 C14 C9 120.9(6) . .
O5 C15 O6 120.2(5) . .
O5 C15 C16 120.2(5) . .
O6 C15 C16 119.6(5) . .
C17 C16 C21 119.5(5) . .
C17 C16 C15 120.8(5) . .
C21 C16 C15 119.7(5) . .
C18 C17 C16 120.2(6) . .
C19 C18 C17 119.6(7) . .
C18 C19 C20 121.6(6) . .
C19 C20 C21 119.3(6) . .
C20 C21 C16 119.7(6) . .
N1 C22 C23 123.0(5) . .
C22 C23 C24 120.7(5) . .
C23 C24 C25 115.6(5) . .
C23 C24 C27 122.9(5) . .
C25 C24 C27 121.5(5) . .
C26 C25 C24 120.4(5) . .
N1 C26 C25 123.5(5) . .
C28 C27 C24 122.7(6) . .
C27 C28 C29 127.7(6) . .
C30 C29 C28 122.0(6) . .
C30 C29 S1 117.3(5) . .
C28 C29 S1 120.7(5) . .
C29 C30 S2 118.8(5) . .
C32 C31 S2 122.3(4) . .
C32 C31 S1 123.0(5) . .
S2 C31 S1 114.7(3) . .
C31 C32 S4 124.3(4) . .
C31 C32 S3 121.4(4) . .
S4 C32 S3 114.2(3) . .
C34 C33 S4 118.7(5) . .
C33 C34 S3 118.5(5) . .
N2 C35 C36 175.2(16) . .
C26 N1 C22 116.7(4) . .
C26 N1 Co2 122.5(3) . .
C22 N1 Co2 120.6(4) . .
C1 O1 Co1 139.8(4) . .
C1 O2 Co2 131.2(4) . .
C8 O3 Co1 139.2(3) . .
C8 O4 Co2 126.2(3) . .
C15 O5 Co1 166.0(3) . .
C15 O5 Co2 83.1(3) . .
Co1 O5 Co2 106.16(15) . .
C15 O6 Co2 98.0(3) . .
C29 S1 C31 94.6(3) . .
C30 S2 C31 94.4(3) . .
C34 S3 C32 93.7(3) . .
C33 S4 C32 94.3(3) . .
O3 Co1 O3 180.000(1) 2_666 .
O3 Co1 O1 86.36(16) 2_666 .
O3 Co1 O1 93.64(16) . .
O3 Co1 O1 93.64(16) 2_666 2_666
O3 Co1 O1 86.36(16) . 2_666
O1 Co1 O1 180.000(1) . 2_666
O3 Co1 O5 90.45(14) 2_666 .
O3 Co1 O5 89.55(14) . .
O1 Co1 O5 90.64(15) . .
O1 Co1 O5 89.36(15) 2_666 .
O3 Co1 O5 89.55(14) 2_666 2_666
O3 Co1 O5 90.45(14) . 2_666
O1 Co1 O5 89.36(15) . 2_666
O1 Co1 O5 90.64(15) 2_666 2_666
O5 Co1 O5 180.00(7) . 2_666
O2 Co2 O4 123.02(16) . .
O2 Co2 O6 112.44(15) . .
O4 Co2 O6 117.55(16) . .
O2 Co2 N1 98.50(17) . .
O4 Co2 N1 98.48(16) . .
O6 Co2 N1 99.62(16) . .
O2 Co2 O5 93.73(14) . .
O4 Co2 O5 90.12(14) . .
O6 Co2 O5 58.47(13) . .
N1 Co2 O5 157.84(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.250(6) .
C1 O2 1.257(6) .
C1 C2 1.516(7) .
C2 C3 1.354(8) .
C2 C7 1.372(8) .
C3 C4 1.383(9) .
C4 C5 1.342(10) .
C5 C6 1.351(10) .
C6 C7 1.398(9) .
C8 O3 1.237(6) .
C8 O4 1.269(6) .
C8 C9 1.499(7) .
C9 C10 1.376(8) .
C9 C14 1.387(7) .
C10 C11 1.402(9) .
C11 C12 1.355(10) .
C12 C13 1.350(10) .
C13 C14 1.382(8) .
C15 O5 1.235(6) .
C15 O6 1.266(6) .
C15 C16 1.489(7) .
C16 C17 1.380(7) .
C16 C21 1.399(7) .
C17 C18 1.374(8) .
C18 C19 1.363(9) .
C19 C20 1.374(9) .
C20 C21 1.376(8) .
C22 N1 1.335(6) .
C22 C23 1.370(7) .
C23 C24 1.383(7) .
C24 C25 1.390(7) .
C24 C27 1.467(7) .
C25 C26 1.365(7) .
C26 N1 1.332(6) .
C27 C28 1.323(8) .
C28 C29 1.472(8) .
C29 C30 1.335(8) .
C29 S1 1.730(7) .
C30 S2 1.724(6) .
C31 C32 1.329(7) .
C31 S2 1.750(6) .
C31 S1 1.765(5) .
C32 S4 1.750(5) .
C32 S3 1.758(6) .
C33 C34 1.317(8) .
C33 S4 1.690(7) .
C34 S3 1.708(7) .
C35 N2 1.122(12) .
C35 C36 1.366(14) .
N1 Co2 2.048(4) .
O1 Co1 2.078(4) .
O2 Co2 1.930(4) .
O3 Co1 2.063(3) .
O4 Co2 1.944(3) .
O5 Co1 2.080(3) .
O5 Co2 2.370(4) .
O6 Co2 2.029(4) .
Co1 O3 2.063(3) 2_666
Co1 O1 2.078(4) 2_666
Co1 O5 2.080(3) 2_666
