Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Francesc Teixidor'
_publ_contact_author_address     
;
Institut de Ciencia de Materials de Barcelona-CSIC
Bellaterra
08193
SPAIN
;

_publ_contact_author_email       TEIXIDOR@ICMAB.ES

_publ_section_title              
;
Polymorphism and phase transformations in
cobaltacarborane molecular crystals: Evidence for very weak
intermolecular C-H...H-B interactions
;
loop_
_publ_author_name
'Francesc Teixidor'
'Jose Giner Planas'
'M. Hursthouse'
'Mark E. Light'
'C. Vinas'

data_2006acc0011
_database_code_depnum_ccdc_archive 'CCDC 642389'

_chemical_compound_source        Pepe

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H16 B9 Co'
_chemical_formula_weight         256.42

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'
B B 0.0013 0.0007 '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   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.0693(2)
_cell_length_b                   9.4904(3)
_cell_length_c                   17.7697(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.844(2)
_cell_angle_gamma                90.00
_cell_volume                     1192.05(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2784
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       'Cut Block'
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8175
_exptl_absorpt_correction_T_max  0.8965
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 11469 reflections reduced R(int) from 0.1360 to 0.0383
Ratio of minimum to maximum apparent transmission: 0.793010
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13433
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.76
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2710
_reflns_number_gt                2384
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.4275P] where P=(Fo^2^+2Fc^2^)/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         2710
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C1 C 0.3996(2) 0.1527(2) 0.19105(10) 0.0143(4) Uani 1 1 d . . .
H1 H 0.5102 0.2287 0.2031 0.017 Uiso 1 1 calc R . .
C2 C 0.1771(3) 0.1903(2) 0.20301(10) 0.0139(4) Uani 1 1 d . . .
H2 H 0.1332 0.2926 0.2234 0.017 Uiso 1 1 calc R . .
C3 C 0.1485(4) 0.4037(2) 0.06419(12) 0.0293(5) Uani 1 1 d . . .
H3 H 0.0476 0.4516 0.0879 0.035 Uiso 1 1 calc R . .
C4 C 0.1293(3) 0.3030(2) 0.00629(12) 0.0238(5) Uani 1 1 d . . .
H4 H 0.0134 0.2716 -0.0156 0.029 Uiso 1 1 calc R . .
C5 C 0.3110(4) 0.2570(3) -0.01352(12) 0.0283(5) Uani 1 1 d . . .
H5 H 0.3398 0.1894 -0.0511 0.034 Uiso 1 1 calc R . .
C6 C 0.4436(4) 0.3301(3) 0.03300(15) 0.0381(6) Uani 1 1 d . . .
H6 H 0.5772 0.3198 0.0321 0.046 Uiso 1 1 calc R . .
C7 C 0.3415(4) 0.4213(3) 0.08090(13) 0.0375(6) Uani 1 1 d . . .
H7 H 0.3944 0.4831 0.1176 0.045 Uiso 1 1 calc R . .
B4 B 0.4305(3) 0.0379(2) 0.11746(12) 0.0154(4) Uani 1 1 d . . .
H4A H 0.5649 0.0324 0.0780 0.018 Uiso 1 1 calc R . .
B5 B 0.4465(3) -0.0171(2) 0.21365(12) 0.0161(4) Uani 1 1 d . . .
H5A H 0.5925 -0.0577 0.2400 0.019 Uiso 1 1 calc R . .
B6 B 0.2878(3) 0.0834(2) 0.26812(12) 0.0161(4) Uani 1 1 d . . .
H6A H 0.3210 0.1143 0.3319 0.019 Uiso 1 1 calc R . .
B7 B 0.0335(3) 0.1047(2) 0.13858(11) 0.0146(4) Uani 1 1 d . . .
H7A H -0.1139 0.1463 0.1140 0.018 Uiso 1 1 calc R . .
B8 B 0.1942(3) -0.0010(2) 0.08309(11) 0.0145(4) Uani 1 1 d . . .
H8 H 0.1610 -0.0358 0.0199 0.017 Uiso 1 1 calc R . .
B9 B 0.3123(3) -0.1184(2) 0.14724(12) 0.0163(4) Uani 1 1 d . . .
H9 H 0.3623 -0.2321 0.1273 0.020 Uiso 1 1 calc R . .
B10 B 0.2248(3) -0.0892(2) 0.23998(12) 0.0162(4) Uani 1 1 d . . .
H10 H 0.2128 -0.1828 0.2843 0.019 Uiso 1 1 calc R . .
B11 B 0.0563(3) 0.0490(2) 0.23473(11) 0.0153(4) Uani 1 1 d . . .
H11 H -0.0745 0.0553 0.2761 0.018 Uiso 1 1 calc R . .
B12 B 0.0687(3) -0.0763(2) 0.16034(11) 0.0148(4) Uani 1 1 d . . .
H12 H -0.0537 -0.1604 0.1495 0.018 Uiso 1 1 calc R . .
Co3 Co 0.26262(3) 0.21352(3) 0.096659(13) 0.01322(12) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0138(9) 0.0138(9) 0.0153(9) 0.0006(7) 0.0009(6) -0.0012(7)
C2 0.0149(9) 0.0138(9) 0.0130(9) 0.0003(7) 0.0014(7) 0.0019(7)
C3 0.0519(15) 0.0158(11) 0.0204(11) 0.0058(8) 0.0028(9) 0.0103(10)
C4 0.0333(12) 0.0214(11) 0.0166(10) 0.0074(8) -0.0031(8) 0.0009(9)
C5 0.0476(14) 0.0211(11) 0.0164(10) 0.0073(8) 0.0120(9) 0.0043(11)
C6 0.0275(12) 0.0436(15) 0.0432(15) 0.0296(12) 0.0010(10) -0.0095(11)
C7 0.0699(18) 0.0178(12) 0.0243(12) 0.0098(9) -0.0155(11) -0.0190(12)
B4 0.0158(10) 0.0131(10) 0.0173(10) -0.0006(8) 0.0041(7) 0.0000(8)
B5 0.0125(9) 0.0160(10) 0.0198(10) 0.0031(8) -0.0007(7) -0.0003(8)
B6 0.0162(10) 0.0187(11) 0.0134(10) 0.0016(8) -0.0006(7) -0.0006(8)
B7 0.0141(10) 0.0170(11) 0.0128(10) 0.0010(7) -0.0006(7) -0.0006(8)
B8 0.0143(10) 0.0144(10) 0.0149(10) -0.0019(8) 0.0019(7) -0.0022(8)
B9 0.0167(10) 0.0127(10) 0.0196(11) 0.0005(8) 0.0024(8) -0.0007(8)
B10 0.0147(10) 0.0164(10) 0.0175(10) 0.0051(8) 0.0001(7) -0.0012(8)
B11 0.0140(10) 0.0172(11) 0.0149(10) 0.0007(8) 0.0005(7) -0.0019(8)
B12 0.0141(10) 0.0152(10) 0.0151(10) 0.0009(8) 0.0005(7) -0.0018(8)
Co3 0.01676(18) 0.01096(18) 0.01196(18) 0.00159(8) 0.00134(11) -0.00087(9)

_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
C1 C2 1.630(3) . ?
C1 B5 1.692(3) . ?
C1 B4 1.719(3) . ?
C1 B6 1.721(3) . ?
C1 Co3 2.0092(18) . ?
C2 B11 1.691(3) . ?
C2 B6 1.718(3) . ?
C2 B7 1.723(3) . ?
C2 Co3 2.0047(18) . ?
C3 C7 1.402(4) . ?
C3 C4 1.409(3) . ?
C3 Co3 2.056(2) . ?
C4 C5 1.406(3) . ?
C4 Co3 2.036(2) . ?
C5 C6 1.422(4) . ?
C5 Co3 2.035(2) . ?
C6 C7 1.418(4) . ?
C6 Co3 2.046(2) . ?
C7 Co3 2.069(2) . ?
B4 B9 1.786(3) . ?
B4 B5 1.789(3) . ?
B4 B8 1.808(3) . ?
B4 Co3 2.076(2) . ?
B5 B6 1.771(3) . ?
B5 B10 1.779(3) . ?
B5 B9 1.784(3) . ?
B6 B11 1.763(3) . ?
B6 B10 1.769(3) . ?
B7 B12 1.778(3) . ?
B7 B11 1.793(3) . ?
B7 B8 1.817(3) . ?
B7 Co3 2.069(2) . ?
B8 B9 1.791(3) . ?
B8 B12 1.794(3) . ?
B8 Co3 2.106(2) . ?
B9 B12 1.786(3) . ?
B9 B10 1.790(3) . ?
B10 B11 1.773(3) . ?
B10 B12 1.786(3) . ?
B11 B12 1.781(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
C2 C1 B5 111.32(14) . . ?
C2 C1 B4 111.82(14) . . ?
B5 C1 B4 63.27(12) . . ?
C2 C1 B6 61.63(11) . . ?
B5 C1 B6 62.50(12) . . ?
B4 C1 B6 115.36(15) . . ?
C2 C1 Co3 65.91(9) . . ?
B5 C1 Co3 124.20(12) . . ?
B4 C1 Co3 67.17(9) . . ?
B6 C1 Co3 123.55(12) . . ?
C1 C2 B11 111.28(15) . . ?
C1 C2 B6 61.81(11) . . ?
B11 C2 B6 62.29(12) . . ?
C1 C2 B7 111.76(14) . . ?
B11 C2 B7 63.38(12) . . ?
B6 C2 B7 115.32(15) . . ?
C1 C2 Co3 66.19(9) . . ?
B11 C2 Co3 124.21(13) . . ?
B6 C2 Co3 123.99(12) . . ?
B7 C2 Co3 66.94(9) . . ?
C7 C3 C4 108.6(2) . . ?
C7 C3 Co3 70.64(13) . . ?
C4 C3 Co3 69.09(12) . . ?
C5 C4 C3 108.4(2) . . ?
C5 C4 Co3 69.74(12) . . ?
C3 C4 Co3 70.63(12) . . ?
C4 C5 C6 107.4(2) . . ?
C4 C5 Co3 69.83(12) . . ?
C6 C5 Co3 70.02(13) . . ?
C7 C6 C5 108.0(2) . . ?
C7 C6 Co3 70.74(13) . . ?
C5 C6 Co3 69.19(13) . . ?
C3 C7 C6 107.6(2) . . ?
C3 C7 Co3 69.61(13) . . ?
C6 C7 Co3 68.94(13) . . ?
C1 B4 B9 103.64(14) . . ?
C1 B4 B5 57.65(11) . . ?
B9 B4 B5 59.87(12) . . ?
C1 B4 B8 105.04(14) . . ?
B9 B4 B8 59.78(12) . . ?
B5 B4 B8 107.95(14) . . ?
C1 B4 Co3 63.11(9) . . ?
B9 B4 Co3 116.80(13) . . ?
B5 B4 Co3 115.61(12) . . ?
B8 B4 Co3 65.24(10) . . ?
C1 B5 B6 59.55(12) . . ?
C1 B5 B10 104.99(14) . . ?
B6 B5 B10 59.77(12) . . ?
C1 B5 B9 104.81(14) . . ?
B6 B5 B9 108.49(14) . . ?
B10 B5 B9 60.33(12) . . ?
C1 B5 B4 59.08(11) . . ?
B6 B5 B4 109.47(15) . . ?
B10 B5 B4 108.66(15) . . ?
B9 B5 B4 59.98(12) . . ?
C2 B6 C1 56.56(11) . . ?
C2 B6 B11 58.10(11) . . ?
C1 B6 B11 103.75(14) . . ?
C2 B6 B10 104.24(14) . . ?
C1 B6 B10 104.21(15) . . ?
B11 B6 B10 60.28(12) . . ?
C2 B6 B5 103.64(14) . . ?
C1 B6 B5 57.95(11) . . ?
B11 B6 B5 107.94(15) . . ?
B10 B6 B5 60.33(12) . . ?
C2 B7 B12 103.39(14) . . ?
C2 B7 B11 57.45(11) . . ?
B12 B7 B11 59.83(12) . . ?
C2 B7 B8 104.70(14) . . ?
B12 B7 B8 59.84(12) . . ?
B11 B7 B8 107.81(15) . . ?
C2 B7 Co3 63.06(9) . . ?
B12 B7 Co3 116.91(13) . . ?
B11 B7 Co3 115.48(12) . . ?
B8 B7 Co3 65.25(9) . . ?
B9 B8 B12 59.76(11) . . ?
B9 B8 B4 59.49(12) . . ?
B12 B8 B4 106.71(14) . . ?
B9 B8 B7 106.69(14) . . ?
B12 B8 B7 58.98(11) . . ?
B4 B8 B7 106.60(14) . . ?
B9 B8 Co3 115.10(12) . . ?
B12 B8 Co3 114.38(12) . . ?
B4 B8 Co3 63.54(9) . . ?
B7 B8 Co3 63.15(9) . . ?
B5 B9 B12 107.30(15) . . ?
B5 B9 B4 60.15(12) . . ?
B12 B9 B4 108.00(15) . . ?
B5 B9 B10 59.69(11) . . ?
B12 B9 B10 59.92(11) . . ?
B4 B9 B10 108.29(15) . . ?
B5 B9 B8 108.92(15) . . ?
B12 B9 B8 60.18(12) . . ?
B4 B9 B8 60.72(12) . . ?
B10 B9 B8 109.01(14) . . ?
B6 B10 B11 59.72(12) . . ?
B6 B10 B5 59.91(12) . . ?
B11 B10 B5 107.17(15) . . ?
B6 B10 B12 108.09(15) . . ?
B11 B10 B12 60.05(12) . . ?
B5 B10 B12 107.55(14) . . ?
B6 B10 B9 108.33(15) . . ?
B11 B10 B9 107.86(14) . . ?
B5 B10 B9 59.99(12) . . ?
B12 B10 B9 59.93(11) . . ?
C2 B11 B6 59.61(12) . . ?
C2 B11 B10 105.18(14) . . ?
B6 B11 B10 60.01(12) . . ?
C2 B11 B12 104.56(14) . . ?
B6 B11 B12 108.53(15) . . ?
B10 B11 B12 60.32(12) . . ?
C2 B11 B7 59.17(11) . . ?
B6 B11 B7 109.62(14) . . ?
B10 B11 B7 108.62(15) . . ?
B12 B11 B7 59.64(11) . . ?
B7 B12 B11 60.53(12) . . ?
B7 B12 B10 108.78(15) . . ?
B11 B12 B10 59.63(11) . . ?
B7 B12 B9 108.67(14) . . ?
B11 B12 B9 107.71(14) . . ?
B10 B12 B9 60.16(12) . . ?
B7 B12 B8 61.18(12) . . ?
B11 B12 B8 109.42(15) . . ?
B10 B12 B8 109.10(14) . . ?
B9 B12 B8 60.06(12) . . ?
C2 Co3 C1 47.91(7) . . ?
C2 Co3 C5 170.62(9) . . ?
C1 Co3 C5 140.89(9) . . ?
C2 Co3 C4 130.31(9) . . ?
C1 Co3 C4 172.03(8) . . ?
C5 Co3 C4 40.43(10) . . ?
C2 Co3 C6 141.31(10) . . ?
C1 Co3 C6 108.63(9) . . ?
C5 Co3 C6 40.79(11) . . ?
C4 Co3 C6 67.93(10) . . ?
C2 Co3 C3 103.80(8) . . ?
C1 Co3 C3 131.98(9) . . ?
C5 Co3 C3 67.84(9) . . ?
C4 Co3 C3 40.28(9) . . ?
C6 Co3 C3 67.42(10) . . ?
C2 Co3 B7 50.00(8) . . ?
C1 Co3 B7 85.77(8) . . ?
C5 Co3 B7 126.24(10) . . ?
C4 Co3 B7 97.84(9) . . ?
C6 Co3 B7 165.60(9) . . ?
C3 Co3 B7 103.48(9) . . ?
C2 Co3 C7 108.55(9) . . ?
C1 Co3 C7 105.03(8) . . ?
C5 Co3 C7 68.11(10) . . ?
C4 Co3 C7 67.56(9) . . ?
C6 Co3 C7 40.32(12) . . ?
C3 Co3 C7 39.75(10) . . ?
B7 Co3 C7 137.59(11) . . ?
C2 Co3 B4 85.60(8) . . ?
C1 Co3 B4 49.72(8) . . ?
C5 Co3 B4 103.32(9) . . ?
C4 Co3 B4 137.08(9) . . ?
C6 Co3 B4 99.92(10) . . ?
C3 Co3 B4 167.33(9) . . ?
B7 Co3 B4 89.06(8) . . ?
C7 Co3 B4 129.40(10) . . ?
C2 Co3 B8 85.96(8) . . ?
C1 Co3 B8 85.68(8) . . ?
C5 Co3 B8 97.32(9) . . ?
C4 Co3 B8 102.13(8) . . ?
C6 Co3 B8 127.18(11) . . ?
C3 Co3 B8 136.72(9) . . ?
B7 Co3 B8 51.60(8) . . ?
C7 Co3 B8 165.41(9) . . ?
B4 Co3 B8 51.23(8) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.070