# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Manuel Almeida'
_publ_contact_author_email       MALMEIDA@ITN.PT

_publ_section_title              
;
Counterion dimerisation effects in the two chain
compound (Per)2Co(mnt)2: Structure and anomalous pressure dependence
of the electrical transport properties
;
loop_
_publ_author_name
'Manuel Almeida'
'James S. Brooks'
'Vasco Gama'
'David Graf'
'Isabel C. Santos'

# Attachment 'PerCo_p21n.cif'

data_p21n
_database_code_depnum_ccdc_archive 'CCDC 710242'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Per2[Co(mnt)2]
;
_chemical_name_common            Per2(Co(mnt)2)
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C20 H12), C8 Co N4 S4'
_chemical_formula_sum            'C48 H24 Co N4 S4'
_chemical_formula_weight         843.88

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.5429(4)
_cell_length_b                   4.06590(10)
_cell_length_c                   25.0320(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0160(10)
_cell_angle_gamma                90.00
_cell_volume                     1784.37(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             862
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_process_details   'SADABS; Sheldrick,2004'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12212
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         28.41
_reflns_number_total             3576
_reflns_number_gt                2278
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The crystals obtained were of poor quality, which results in a weak data set
and low fraction (0.795) of measured theta full.

Due to problems with substantial anisotropy on the S2 Sulfur
atom, disorder model was applied and the S2 atom was refined
over two position (S2-S3) with s.o.f. 50:50.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0221P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3576
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_restrained_S_all      0.822
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.50064(4) 0.39190(12) 0.49137(2) 0.02124(14) Uani 0.50 1 d P . .
S1 S 0.38778(4) 0.46408(17) 0.46245(2) 0.03740(17) Uani 1 1 d . . .
S2 S 0.46970(7) 0.2630(7) 0.57121(7) 0.0274(6) Uani 0.505(5) 1 d P . 1
S3 S 0.46652(7) 0.0899(7) 0.55861(6) 0.0221(5) Uani 0.495(5) 1 d P . 2
C1 C 0.33726(14) 0.2526(6) 0.50900(9) 0.0301(5) Uani 1 1 d . . .
C2 C 0.37189(15) 0.1297(6) 0.55436(9) 0.0324(5) Uani 1 1 d . . .
C3 C 0.25698(17) 0.2072(6) 0.49868(10) 0.0375(6) Uani 1 1 d . . .
C4 C 0.33238(16) -0.0534(6) 0.59363(9) 0.0351(6) Uani 1 1 d . . .
C10 C 0.54762(12) 0.6856(4) 0.17453(8) 0.0211(4) Uani 1 1 d . . .
C11 C 0.54558(12) 0.5995(4) 0.22963(8) 0.0202(4) Uani 1 1 d . . .
C12 C 0.60234(13) 0.7217(5) 0.26468(8) 0.0247(5) Uani 1 1 d . . .
H12 H 0.6013 0.6649 0.3015 0.030 Uiso 1 1 calc R . .
C13 C 0.66032(13) 0.9237(5) 0.24744(9) 0.0267(5) Uani 1 1 d . . .
H13 H 0.6978 1.0052 0.2724 0.032 Uiso 1 1 calc R . .
C14 C 0.66357(13) 1.0061(5) 0.19428(9) 0.0269(5) Uani 1 1 d . . .
H14 H 0.7035 1.1439 0.1827 0.032 Uiso 1 1 calc R . .
C15 C 0.60811(13) 0.8878(5) 0.15667(9) 0.0236(4) Uani 1 1 d . . .
C16 C 0.61134(14) 0.9700(5) 0.10219(9) 0.0287(5) Uani 1 1 d . . .
H16 H 0.6517 1.1040 0.0903 0.034 Uiso 1 1 calc R . .
C17 C 0.55683(14) 0.8584(5) 0.06627(9) 0.0307(5) Uani 1 1 d . . .
H17 H 0.5598 0.9147 0.0296 0.037 Uiso 1 1 calc R . .
C18 C 0.49722(14) 0.6638(5) 0.08290(9) 0.0269(5) Uani 1 1 d . . .
H18 H 0.4597 0.5902 0.0574 0.032 Uiso 1 1 calc R . .
C19 C 0.49119(12) 0.5732(4) 0.13670(8) 0.0203(4) Uani 1 1 d . . .
C20 C 0.42878(13) 0.3678(5) 0.15483(8) 0.0215(4) Uani 1 1 d . . .
C21 C 0.37111(13) 0.2523(5) 0.11994(9) 0.0267(5) Uani 1 1 d . . .
H21 H 0.3724 0.3077 0.0831 0.032 Uiso 1 1 calc R . .
C22 C 0.31183(14) 0.0579(5) 0.13762(10) 0.0304(5) Uani 1 1 d . . .
H22 H 0.2725 -0.0120 0.1131 0.036 Uiso 1 1 calc R . .
C23 C 0.31006(13) -0.0328(5) 0.19027(10) 0.0284(5) Uani 1 1 d . . .
H23 H 0.2703 -0.1716 0.2017 0.034 Uiso 1 1 calc R . .
C24 C 0.36617(13) 0.0763(5) 0.22761(9) 0.0245(5) Uani 1 1 d . . .
C25 C 0.36441(13) -0.0115(5) 0.28195(9) 0.0277(5) Uani 1 1 d . . .
H25 H 0.3248 -0.1499 0.2938 0.033 Uiso 1 1 calc R . .
C26 C 0.41904(14) 0.0995(5) 0.31811(9) 0.0300(5) Uani 1 1 d . . .
H26 H 0.4163 0.0416 0.3548 0.036 Uiso 1 1 calc R . .
C27 C 0.47856(14) 0.2971(5) 0.30132(9) 0.0263(5) Uani 1 1 d . . .
H27 H 0.5164 0.3695 0.3268 0.032 Uiso 1 1 calc R . .
C28 C 0.48387(12) 0.3912(4) 0.24791(8) 0.0206(4) Uani 1 1 d . . .
C29 C 0.42702(12) 0.2801(4) 0.20978(8) 0.0198(4) Uani 1 1 d . . .
N1 N 0.19268(16) 0.1745(6) 0.49062(9) 0.0563(7) Uani 1 1 d . . .
N2 N 0.30318(16) -0.2016(6) 0.62538(9) 0.0531(7) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 S1 2.1046(9) . ?
Co1 S2 2.1540(14) . ?
Co1 S2 2.1796(15) 3_666 ?
Co1 S3 2.1841(15) . ?
Co1 S1 2.3133(9) 3_666 ?
Co1 S3 2.405(3) 3_656 ?
Co1 S3 2.527(2) 3_666 ?
S1 C1 1.719(3) . ?
S1 Co1 2.3133(9) 3_666 ?
S2 C2 1.834(3) . ?
S2 Co1 2.1796(15) 3_666 ?
S3 C2 1.668(3) . ?
S3 Co1 2.405(3) 3_656 ?
S3 Co1 2.527(2) 3_666 ?
C1 C2 1.364(3) . ?
C1 C3 1.435(4) . ?
C2 C4 1.431(3) . ?
C3 N1 1.147(4) . ?
C4 N2 1.134(3) . ?
C10 C19 1.421(3) . ?
C10 C11 1.425(3) . ?
C10 C15 1.427(3) . ?
C11 C12 1.395(3) . ?
C11 C28 1.461(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.375(3) . ?
C14 C15 1.414(3) . ?
C15 C16 1.407(3) . ?
C16 C17 1.367(3) . ?
C17 C18 1.387(3) . ?
C18 C19 1.404(3) . ?
C19 C20 1.462(3) . ?
C20 C21 1.395(3) . ?
C20 C29 1.422(3) . ?
C21 C22 1.391(3) . ?
C22 C23 1.370(3) . ?
C23 C24 1.405(3) . ?
C24 C25 1.408(3) . ?
C24 C29 1.435(3) . ?
C25 C26 1.371(3) . ?
C26 C27 1.394(3) . ?
C27 C28 1.397(3) . ?
C28 C29 1.429(3) . ?

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
_geom_angle_publ_flag
Co1 Co1 S1 89.46(7) 3_666 . ?
Co1 Co1 S2 78.39(11) 3_666 . ?
S1 Co1 S2 95.07(4) . . ?
Co1 Co1 S2 75.48(10) 3_666 3_666 ?
S1 Co1 S2 84.75(4) . 3_666 ?
S2 Co1 S2 153.87(3) . 3_666 ?
Co1 Co1 S3 98.82(10) 3_666 . ?
S1 Co1 S3 93.63(4) . . ?
S2 Co1 S3 20.50(4) . . ?
S2 Co1 S3 174.06(5) 3_666 . ?
Co1 Co1 S1 65.47(7) 3_666 3_666 ?
S1 Co1 S1 154.93(3) . 3_666 ?
S2 Co1 S1 80.47(6) . 3_666 ?
S2 Co1 S1 88.68(6) 3_666 3_666 ?
S3 Co1 S1 90.42(5) . 3_666 ?
Co1 Co1 S3 165.79(9) 3_666 3_656 ?
S1 Co1 S3 100.04(4) . 3_656 ?
S2 Co1 S3 110.93(7) . 3_656 ?
S2 Co1 S3 94.76(7) 3_666 3_656 ?
S3 Co1 S3 91.15(7) . 3_656 ?
S1 Co1 S3 104.60(4) 3_666 3_656 ?
Co1 Co1 S3 58.65(8) 3_666 3_666 ?
S1 Co1 S3 86.65(4) . 3_666 ?
S2 Co1 S3 137.01(5) . 3_666 ?
S2 Co1 S3 16.90(5) 3_666 3_666 ?
S3 Co1 S3 157.47(4) . 3_666 ?
S1 Co1 S3 80.37(4) 3_666 3_666 ?
S3 Co1 S3 111.01(6) 3_656 3_666 ?
C1 S1 Co1 101.44(9) . . ?
C1 S1 Co1 103.61(9) . 3_666 ?
Co1 S1 Co1 25.07(3) . 3_666 ?
C2 S2 Co1 97.05(11) . . ?
C2 S2 Co1 105.66(9) . 3_666 ?
Co1 S2 Co1 26.13(3) . 3_666 ?
C2 S3 Co1 101.27(10) . . ?
C2 S3 Co1 107.58(15) . 3_656 ?
Co1 S3 Co1 88.85(7) . 3_656 ?
C2 S3 Co1 97.54(12) . 3_666 ?
Co1 S3 Co1 22.53(4) . 3_666 ?
Co1 S3 Co1 111.01(6) 3_656 3_666 ?
C2 C1 C3 120.6(2) . . ?
C2 C1 S1 121.5(2) . . ?
C3 C1 S1 117.94(18) . . ?
C1 C2 C4 123.4(2) . . ?
C1 C2 S3 120.13(19) . . ?
C4 C2 S3 114.25(19) . . ?
C1 C2 S2 117.96(19) . . ?
C4 C2 S2 117.87(18) . . ?
S3 C2 S2 24.90(6) . . ?
N1 C3 C1 179.2(3) . . ?
N2 C4 C2 177.9(3) . . ?
C19 C10 C11 121.7(2) . . ?
C19 C10 C15 119.00(19) . . ?
C11 C10 C15 119.28(19) . . ?
C12 C11 C10 118.7(2) . . ?
C12 C11 C28 121.99(19) . . ?
C10 C11 C28 119.33(19) . . ?
C13 C12 C11 122.0(2) . . ?
C14 C13 C12 120.1(2) . . ?
C13 C14 C15 120.7(2) . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 C10 119.7(2) . . ?
C14 C15 C10 119.3(2) . . ?
C17 C16 C15 120.5(2) . . ?
C16 C17 C18 120.6(2) . . ?
C17 C18 C19 121.4(2) . . ?
C18 C19 C10 118.7(2) . . ?
C18 C19 C20 122.02(19) . . ?
C10 C19 C20 119.24(18) . . ?
C21 C20 C29 118.8(2) . . ?
C21 C20 C19 122.20(19) . . ?
C29 C20 C19 119.04(19) . . ?
C22 C21 C20 121.8(2) . . ?
C23 C22 C21 120.1(2) . . ?
C22 C23 C24 121.1(2) . . ?
C23 C24 C25 121.6(2) . . ?
C23 C24 C29 119.1(2) . . ?
C25 C24 C29 119.3(2) . . ?
C26 C25 C24 121.0(2) . . ?
C25 C26 C27 120.3(2) . . ?
C26 C27 C28 121.5(2) . . ?
C27 C28 C29 119.0(2) . . ?
C27 C28 C11 122.26(19) . . ?
C29 C28 C11 118.77(18) . . ?
C20 C29 C28 121.9(2) . . ?
C20 C29 C24 119.16(19) . . ?
C28 C29 C24 118.95(19) . . ?

_diffrn_measured_fraction_theta_max 0.795
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.795
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.049

# start Validation Reply Form
_vrf_REFLT03_p21n                
;
PROBLEM: Reflection count < 85% complete (theta max?)
RESPONSE:The crystals obtained were of poor quality, which results
in a weak data set
and low fraction (0.795) of measured theta full.
;
_vrf_PLAT029_p21n                
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.80
RESPONSE: The crystals obtained were of poor quality, which results
in a weak data set
and low fraction (0.795) of measured theta full.
;
# end Validation Reply Form



