#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180118 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/16/7101648.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_7101648
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 Co2 Mn N4 O12 S8'
_chemical_formula_weight         1596.47
_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                95.5940(10)
_cell_angle_beta                 106.8340(11)
_cell_angle_gamma                90.2950(12)
_cell_formula_units_Z            1
_cell_length_a                   10.6124(3)
_cell_length_b                   11.7260(3)
_cell_length_c                   14.9724(5)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1773.76(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14183
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       losange
_exptl_crystal_F_000             817
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         8135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0436
_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)+(0.0487P)²+1.0328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                6262
_reflns_number_total             8135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613191c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101648
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 0.4034(3) 0.2334(2) 0.45897(19) 0.0369(5) Uani 1 1 d .
C2 C 0.4067(3) 0.1269(2) 0.3947(2) 0.0400(6) Uani 1 1 d .
C3 C 0.4580(4) 0.1338(3) 0.3209(2) 0.0567(8) Uani 1 1 d .
H3 H 0.4893 0.2041 0.3107 0.068 Uiso 1 1 calc R
C4 C 0.4634(4) 0.0362(3) 0.2613(3) 0.0651(9) Uani 1 1 d .
H4 H 0.4985 0.0413 0.2116 0.078 Uiso 1 1 calc R
C5 C 0.4169(4) -0.0677(3) 0.2761(3) 0.0605(9) Uani 1 1 d .
H5 H 0.4203 -0.1328 0.2362 0.073 Uiso 1 1 calc R
C6 C 0.3655(3) -0.0758(3) 0.3492(3) 0.0600(9) Uani 1 1 d .
H6 H 0.3344 -0.1464 0.3590 0.072 Uiso 1 1 calc R
C7 C 0.3596(3) 0.0219(2) 0.4095(2) 0.0482(7) Uani 1 1 d .
H7 H 0.3244 0.0164 0.4591 0.058 Uiso 1 1 calc R
C8 C 0.2325(2) 0.5400(2) 0.55346(18) 0.0355(5) Uani 1 1 d .
C9 C 0.1414(2) 0.6374(2) 0.55344(19) 0.0366(5) Uani 1 1 d .
C10 C 0.1583(3) 0.7354(3) 0.5124(2) 0.0479(7) Uani 1 1 d .
H10 H 0.2247 0.7399 0.4836 0.057 Uiso 1 1 calc R
C11 C 0.0759(3) 0.8264(3) 0.5146(3) 0.0574(8) Uani 1 1 d .
H11 H 0.0885 0.8928 0.4885 0.069 Uiso 1 1 calc R
C12 C -0.0240(3) 0.8190(3) 0.5550(2) 0.0546(8) Uani 1 1 d .
H12 H -0.0798 0.8799 0.5551 0.066 Uiso 1 1 calc R
C13 C -0.0425(3) 0.7227(3) 0.5952(2) 0.0508(7) Uani 1 1 d .
H13 H -0.1103 0.7183 0.6228 0.061 Uiso 1 1 calc R
C14 C 0.0406(3) 0.6316(3) 0.5947(2) 0.0439(6) Uani 1 1 d .
H14 H 0.0284 0.5662 0.6222 0.053 Uiso 1 1 calc R
C15 C 0.5741(3) 0.4046(2) 0.71221(17) 0.0337(5) Uani 1 1 d .
C16 C 0.7133(3) 0.4283(2) 0.76829(18) 0.0360(5) Uani 1 1 d .
C17 C 0.7918(3) 0.5038(3) 0.7396(2) 0.0445(6) Uani 1 1 d .
H17 H 0.7574 0.5383 0.6847 0.053 Uiso 1 1 calc R
C18 C 0.9208(3) 0.5272(3) 0.7928(2) 0.0504(7) Uani 1 1 d .
H18 H 0.9730 0.5785 0.7742 0.061 Uiso 1 1 calc R
C19 C 0.9724(3) 0.4748(3) 0.8734(2) 0.0523(7) Uani 1 1 d .
H19 H 1.0597 0.4902 0.9085 0.063 Uiso 1 1 calc R
C20 C 0.8950(3) 0.3990(3) 0.9028(2) 0.0479(7) Uani 1 1 d .
H20 H 0.9304 0.3638 0.9572 0.057 Uiso 1 1 calc R
C21 C 0.7649(3) 0.3764(2) 0.85046(19) 0.0390(6) Uani 1 1 d .
H21 H 0.7121 0.3267 0.8701 0.047 Uiso 1 1 calc R
C22 C 0.1273(3) 0.2782(2) 0.7128(2) 0.0446(6) Uani 1 1 d .
H22 H 0.1154 0.3566 0.7109 0.053 Uiso 1 1 calc R
C23 C 0.0526(3) 0.2181(3) 0.7543(2) 0.0481(7) Uani 1 1 d .
H23 H -0.0090 0.2555 0.7789 0.058 Uiso 1 1 calc R
C24 C 0.0689(3) 0.1003(2) 0.7596(2) 0.0400(6) Uani 1 1 d .
C25 C 0.1590(3) 0.0497(2) 0.7175(2) 0.0401(6) Uani 1 1 d .
H25 H 0.1715 -0.0288 0.7173 0.048 Uiso 1 1 calc R
C26 C 0.2294(3) 0.1158(2) 0.67643(19) 0.0384(6) Uani 1 1 d .
H26 H 0.2885 0.0801 0.6484 0.046 Uiso 1 1 calc R
C27 C -0.0047(3) 0.0336(2) 0.8070(2) 0.0430(6) Uani 1 1 d .
H27 H -0.0093 -0.0459 0.7947 0.052 Uiso 1 1 calc R
C28 C -0.0652(3) 0.0817(3) 0.8668(2) 0.0457(6) Uani 1 1 d .
H28 H -0.0553 0.1610 0.8793 0.055 Uiso 1 1 calc R
C29 C -0.1447(3) 0.0254(3) 0.9150(2) 0.0439(6) Uani 1 1 d .
C30 C -0.2057(3) 0.0841(3) 0.9702(2) 0.0475(7) Uani 1 1 d .
H30 H -0.1932 0.1632 0.9828 0.057 Uiso 1 1 calc R
C31 C -0.2702(3) -0.1248(2) 0.9752(2) 0.0409(6) Uani 1 1 d .
C32 C -0.3126(3) -0.2222(2) 0.9977(2) 0.0400(6) Uani 1 1 d .
C33 C -0.3977(3) -0.3739(3) 1.0790(2) 0.0517(7) Uani 1 1 d .
H33 H -0.4323 -0.4111 1.1192 0.062 Uiso 1 1 calc R
C34 C -0.3369(3) -0.4315(3) 1.0242(2) 0.0518(7) Uani 1 1 d .
H34 H -0.3280 -0.5103 1.0247 0.062 Uiso 1 1 calc R
C35 C 0.7178(4) 0.3146(3) 0.1522(3) 0.0632(9) Uani 1 1 d .
C36 C 0.6285(5) 0.3149(6) 0.2075(3) 0.1047(18) Uani 1 1 d .
H36A H 0.6197 0.3921 0.2325 0.157 Uiso 1 1 calc R
H36B H 0.6617 0.2686 0.2582 0.157 Uiso 1 1 calc R
H36C H 0.5440 0.2843 0.1691 0.157 Uiso 1 1 calc R
N1 N 0.2166(2) 0.22999(19) 0.67495(16) 0.0375(5) Uani 1 1 d .
N2 N 0.7873(4) 0.3149(3) 0.1072(3) 0.0860(11) Uani 1 1 d .
O1 O 0.4437(2) 0.32599(17) 0.44043(15) 0.0525(5) Uani 1 1 d .
O2 O 0.35834(18) 0.21988(15) 0.52701(13) 0.0394(4) Uani 1 1 d .
O3 O 0.30134(19) 0.53668(19) 0.49888(14) 0.0467(5) Uani 1 1 d .
O4 O 0.23116(18) 0.46564(16) 0.61053(14) 0.0407(4) Uani 1 1 d .
O5 O 0.52857(18) 0.44464(18) 0.63578(13) 0.0443(5) Uani 1 1 d .
O6 O 0.50009(18) 0.34158(15) 0.74177(13) 0.0383(4) Uani 1 1 d .
S1 S -0.17111(7) -0.12363(6) 0.89862(6) 0.04604(18) Uani 1 1 d .
S2 S -0.30848(8) 0.01132(6) 1.01823(6) 0.04869(19) Uani 1 1 d .
S3 S -0.27415(8) -0.35656(6) 0.95170(6) 0.04767(18) Uani 1 1 d .
S4 S -0.41123(7) -0.22798(6) 1.07403(5) 0.04423(17) Uani 1 1 d .
Co2 Co 0.33881(3) 0.32995(3) 0.62771(2) 0.03456(10) Uani 1 1 d .
Mn1 Mn 0.5000 0.5000 0.5000 0.03172(13) Uani 1 2 d S
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'
Mn Mn 0.3368 0.7283 '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 126.1(2) . .
O1 C1 C2 117.9(2) . .
O2 C1 C2 115.9(2) . .
C3 C2 C7 119.6(3) . .
C3 C2 C1 119.5(3) . .
C7 C2 C1 120.9(3) . .
C2 C3 C4 120.5(3) . .
C5 C4 C3 119.8(3) . .
C6 C5 C4 120.3(3) . .
C5 C6 C7 120.2(3) . .
C2 C7 C6 119.5(3) . .
O3 C8 O4 125.4(2) . .
O3 C8 C9 118.6(2) . .
O4 C8 C9 116.0(2) . .
C14 C9 C10 119.2(3) . .
C14 C9 C8 120.8(2) . .
C10 C9 C8 120.0(2) . .
C11 C10 C9 119.8(3) . .
C12 C11 C10 120.3(3) . .
C13 C12 C11 120.6(3) . .
C12 C13 C14 119.6(3) . .
C9 C14 C13 120.5(3) . .
O5 C15 O6 119.3(2) . .
O5 C15 C16 120.9(2) . .
O6 C15 C16 119.8(2) . .
C17 C16 C21 120.1(3) . .
C17 C16 C15 119.9(2) . .
C21 C16 C15 120.0(2) . .
C18 C17 C16 119.8(3) . .
C19 C18 C17 120.2(3) . .
C18 C19 C20 120.6(3) . .
C21 C20 C19 119.5(3) . .
C20 C21 C16 119.8(3) . .
N1 C22 C23 123.4(3) . .
C22 C23 C24 119.9(3) . .
C25 C24 C23 116.5(2) . .
C25 C24 C27 121.7(3) . .
C23 C24 C27 121.8(3) . .
C26 C25 C24 120.0(3) . .
N1 C26 C25 122.9(2) . .
C28 C27 C24 122.9(3) . .
C27 C28 C29 127.9(3) . .
C30 C29 C28 122.2(3) . .
C30 C29 S1 116.7(2) . .
C28 C29 S1 121.0(2) . .
C29 C30 S2 119.3(2) . .
C32 C31 S2 123.1(2) . .
C32 C31 S1 122.0(2) . .
S2 C31 S1 114.86(16) . .
C31 C32 S3 121.7(2) . .
C31 C32 S4 123.7(2) . .
S3 C32 S4 114.56(15) . .
C34 C33 S4 118.3(2) . .
C33 C34 S3 118.3(3) . .
N2 C35 C36 179.0(5) . .
C22 N1 C26 117.1(2) . .
C22 N1 Co2 120.49(18) . .
C26 N1 Co2 122.15(17) . .
C1 O1 Mn1 141.76(19) . .
C1 O2 Co2 130.41(17) . .
C8 O3 Mn1 138.73(18) . .
C8 O4 Co2 125.85(16) . .
C15 O5 Mn1 164.65(18) . .
C15 O5 Co2 83.27(15) . .
Mn1 O5 Co2 106.78(8) . .
C15 O6 Co2 98.81(16) . .
C29 S1 C31 94.46(13) . .
C30 S2 C31 94.14(14) . .
C34 S3 C32 93.94(14) . .
C33 S4 C32 93.91(14) . .
O2 Co2 O4 125.17(8) . .
O2 Co2 O6 112.39(8) . .
O4 Co2 O6 116.28(8) . .
O2 Co2 N1 97.49(8) . .
O4 Co2 N1 98.05(8) . .
O6 Co2 N1 99.42(8) . .
O2 Co2 O5 94.99(7) . .
O4 Co2 O5 89.94(7) . .
O6 Co2 O5 58.31(7) . .
N1 Co2 O5 157.43(8) . .
O5 Mn1 O5 180.00(4) . 2_666
O5 Mn1 O3 87.55(7) . .
O5 Mn1 O3 92.45(7) 2_666 .
O5 Mn1 O3 92.45(7) . 2_666
O5 Mn1 O3 87.55(7) 2_666 2_666
O3 Mn1 O3 180.00(11) . 2_666
O5 Mn1 O1 91.37(8) . 2_666
O5 Mn1 O1 88.63(8) 2_666 2_666
O3 Mn1 O1 88.31(9) . 2_666
O3 Mn1 O1 91.69(9) 2_666 2_666
O5 Mn1 O1 88.63(8) . .
O5 Mn1 O1 91.37(8) 2_666 .
O3 Mn1 O1 91.69(9) . .
O3 Mn1 O1 88.31(9) 2_666 .
O1 Mn1 O1 180.0 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.249(3) .
C1 O2 1.267(3) .
C1 C2 1.508(4) .
C2 C3 1.373(4) .
C2 C7 1.387(4) .
C3 C4 1.394(4) .
C4 C5 1.373(5) .
C5 C6 1.368(5) .
C6 C7 1.401(4) .
C8 O3 1.242(3) .
C8 O4 1.282(3) .
C8 C9 1.500(3) .
C9 C14 1.387(4) .
C9 C10 1.388(4) .
C10 C11 1.388(4) .
C11 C12 1.371(5) .
C12 C13 1.370(5) .
C13 C14 1.389(4) .
C15 O5 1.245(3) .
C15 O6 1.272(3) .
C15 C16 1.482(4) .
C16 C17 1.391(4) .
C16 C21 1.394(4) .
C17 C18 1.381(4) .
C18 C19 1.378(5) .
C19 C20 1.391(5) .
C20 C21 1.386(4) .
C22 N1 1.340(3) .
C22 C23 1.370(4) .
C23 C24 1.400(4) .
C24 C25 1.395(4) .
C24 C27 1.466(4) .
C25 C26 1.375(4) .
C26 N1 1.349(3) .
C27 C28 1.331(4) .
C28 C29 1.452(4) .
C29 C30 1.334(4) .
C29 S1 1.750(3) .
C30 S2 1.731(3) .
C31 C32 1.332(4) .
C31 S2 1.757(3) .
C31 S1 1.767(3) .
C32 S3 1.755(3) .
C32 S4 1.765(3) .
C33 C34 1.322(4) .
C33 S4 1.725(3) .
C34 S3 1.730(3) .
C35 N2 1.135(5) .
C35 C36 1.427(6) .
N1 Co2 2.057(2) .
O1 Mn1 2.1541(19) .
O2 Co2 1.9459(19) .
O3 Mn1 2.1495(18) .
O4 Co2 1.9573(18) .
O5 Mn1 2.1327(18) .
O5 Co2 2.383(2) .
O6 Co2 2.0307(19) .
Mn1 O5 2.1327(18) 2_666
Mn1 O3 2.1495(18) 2_666
Mn1 O1 2.154(2) 2_666
