# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002
data_[Co(C5H4COOH)(C5H4COO)]2.K+Br-

_database_code_CSD	191071



_journal_coden_Cambridge      182


loop_
_publ_author_name
'Dario Braga'
'Fabrizia Grepioni'
'Lucia Maini'
'Marco Polito'

_publ_contact_author_name     	'Prof Dario Braga'  
_publ_contact_author_address 
;
Dipartimento di Chimica G. Ciamician
University of Bologna
Via Selmi 2
Bologna
40126
ITALY
;

_publ_contact_author_email       'DBRAGA@CIAM.UNIBO.IT'

_publ_requested_journal       'Chemical Communications'


_publ_section_title		
;
Unexpected Solid-Solid Reaction upon Preparation of KBr
Pellets and its Exploitation in Supramolecular Cation Complexation
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C24 H18 Br Co2 K O8' 
_chemical_formula_weight          671.25 

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' 
'Br'  'Br'  -0.2901   2.4595 
'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' 
'K'  'K'   0.2009   0.2494 
'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' 

_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1 

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, -y, -z' 

_cell_length_a                    5.9850(10) 
_cell_length_b                    8.096(2) 
_cell_length_c                    12.614(2) 
_cell_angle_alpha                 78.28(2) 
_cell_angle_beta                  80.15(2) 
_cell_angle_gamma                 73.62(2) 
_cell_volume                      569.95(19) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        prism 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.956 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              334 
_exptl_absorpt_coefficient_mu     3.442 
_exptl_absorpt_correction_type    Psi-scan 
_exptl_absorpt_correction_T_min   0.4163 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2077 
_diffrn_reflns_av_R_equivalents   0.0194 
_diffrn_reflns_av_sigmaI/netI     0.0258 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          5.17 
_diffrn_reflns_theta_max          24.97 
_reflns_number_total              1983 
_reflns_number_gt                 1583 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0639P)^2^+0.1357P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1983 
_refine_ls_number_parameters      148 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0480 
_refine_ls_R_factor_gt            0.0316 
_refine_ls_wR_factor_ref          0.0901 
_refine_ls_wR_factor_gt           0.0826 
_refine_ls_goodness_of_fit_ref    1.006 
_refine_ls_restrained_S_all       1.006 
_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 0.82003(7) -0.29583(5) 0.71473(3) 0.02100(16) Uani 1 1 d . . . 
C1 C 0.6545(3) -0.4801(3) 0.7954(2) 0.0356(8) Uani 1 1 d G . . 
H1A H 0.4919 -0.4793 0.7918 0.043 Uiso 1 1 calc R . . 
C2 C 0.8545(4) -0.5562(3) 0.72635(18) 0.0373(8) Uani 1 1 d G . . 
H2A H 0.8541 -0.6164 0.6664 0.045 Uiso 1 1 calc R . . 
C3 C 1.0549(3) -0.5278(3) 0.7586(2) 0.0372(9) Uani 1 1 d G . . 
H3A H 1.2170 -0.5648 0.7246 0.045 Uiso 1 1 calc R . . 
C4 C 0.9788(4) -0.4343(3) 0.84752(19) 0.0323(8) Uani 1 1 d G . . 
H4A H 1.0792 -0.3957 0.8859 0.039 Uiso 1 1 calc R . . 
C5 C 0.7313(4) -0.4048(3) 0.87030(17) 0.0288(7) Uani 1 1 d G . . 
C6 C 0.5708(6) -0.3055(4) 0.9542(3) 0.0303(8) Uani 1 1 d . . . 
O1 O 0.6762(4) -0.2501(3) 1.0149(2) 0.0402(6) Uani 1 1 d . . . 
O2 O 0.3599(4) -0.2856(3) 0.9596(2) 0.0407(6) Uani 1 1 d . . . 
C7 C 0.5905(3) -0.1176(3) 0.6205(2) 0.0358(8) Uani 1 1 d G . . 
H7A H 0.4294 -0.1201 0.6164 0.043 Uiso 1 1 calc R . . 
C8 C 0.7945(4) -0.1969(3) 0.55482(17) 0.0367(8) Uani 1 1 d G . . 
H8A H 0.7990 -0.2634 0.4973 0.044 Uiso 1 1 calc R . . 
C9 C 0.9911(3) -0.1638(3) 0.58759(19) 0.0344(8) Uani 1 1 d G . . 
H9A H 1.1551 -0.2037 0.5568 0.041 Uiso 1 1 calc R . . 
C10 C 0.9086(4) -0.0641(3) 0.67348(19) 0.0324(8) Uani 1 1 d G . . 
H10A H 1.0058 -0.0235 0.7125 0.039 Uiso 1 1 calc R . . 
C11 C 0.6610(4) -0.0356(3) 0.69379(17) 0.0288(7) Uani 1 1 d G . . 
C12 C 0.4993(6) 0.0529(4) 0.7817(3) 0.0311(8) Uani 1 1 d . . . 
O3 O 0.6015(5) 0.1113(3) 0.8418(2) 0.0412(6) Uani 1 1 d . . . 
O4 O 0.2883(5) 0.0641(4) 0.7902(3) 0.0454(7) Uani 1 1 d . . . 
K1 K 0.0000 0.0000 1.0000 0.0496(4) Uani 1 2 d S . . 
Br1 Br 0.5000 0.5000 0.5000 0.0544(2) Uani 1 2 d S . . 
H300 H 0.4782 0.1628 0.9011 0.0900 Uiso 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 
Co1 0.0240(2) 0.0185(2) 0.0192(2) 0.00198(16) -0.00412(16) -0.00615(16) 
C1 0.041(2) 0.0287(18) 0.037(2) -0.0001(15) -0.0004(16) -0.0161(15) 
C2 0.052(2) 0.0220(17) 0.035(2) -0.0030(15) -0.0033(17) -0.0079(16) 
C3 0.043(2) 0.0243(17) 0.033(2) -0.0008(15) -0.0059(16) 0.0079(15) 
C4 0.0363(18) 0.0279(17) 0.0252(17) 0.0010(14) -0.0083(14) 0.0029(14) 
C5 0.0368(18) 0.0207(16) 0.0233(17) 0.0058(13) -0.0031(14) -0.0053(14) 
C6 0.0366(19) 0.0225(16) 0.0223(17) 0.0067(13) -0.0024(14) -0.0007(14) 
O1 0.0413(14) 0.0447(15) 0.0314(14) -0.0091(12) -0.0030(11) -0.0045(12) 
O2 0.0358(14) 0.0419(15) 0.0387(15) -0.0020(12) -0.0004(11) -0.0065(12) 
C7 0.0356(18) 0.0370(19) 0.0293(19) 0.0042(15) -0.0133(15) -0.0020(15) 
C8 0.052(2) 0.0359(19) 0.0192(17) 0.0020(15) -0.0062(15) -0.0093(17) 
C9 0.042(2) 0.0271(17) 0.0300(19) 0.0031(14) 0.0058(15) -0.0127(15) 
C10 0.0378(18) 0.0238(16) 0.035(2) -0.0037(14) 0.0050(15) -0.0128(14) 
C11 0.0378(18) 0.0200(16) 0.0228(17) 0.0057(13) -0.0037(14) -0.0048(14) 
C12 0.0344(19) 0.0172(15) 0.0333(19) 0.0022(14) 0.0005(15) -0.0006(14) 
O3 0.0420(14) 0.0420(15) 0.0399(15) -0.0153(12) 0.0045(12) -0.0108(12) 
O4 0.0365(15) 0.0387(15) 0.0573(18) -0.0108(13) -0.0015(13) -0.0043(12) 
K1 0.0368(6) 0.0411(7) 0.0592(8) -0.0054(6) 0.0063(6) -0.0004(5) 
Br1 0.0375(3) 0.0726(4) 0.0626(4) -0.0389(3) -0.0025(3) -0.0119(3) 

_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 C8 2.028(2) . ? 
Co1 C1 2.029(2) . ? 
Co1 C9 2.030(2) . ? 
Co1 C5 2.029(2) . ? 
Co1 C7 2.032(2) . ? 
Co1 C2 2.036(2) . ? 
Co1 C10 2.035(2) . ? 
Co1 C11 2.036(2) . ? 
Co1 C4 2.036(2) . ? 
Co1 C3 2.041(2) . ? 
C1 C2 1.4200 . ? 
C1 C5 1.4200 . ? 
C1 H1A 0.9800 . ? 
C2 C3 1.4200 . ? 
C2 H2A 0.9800 . ? 
C3 C4 1.4200 . ? 
C3 H3A 0.9800 . ? 
C4 C5 1.4200 . ? 
C4 H4A 0.9800 . ? 
C5 C6 1.501(4) . ? 
C6 O2 1.218(4) . ? 
C6 O1 1.285(5) . ? 
O1 K1 3.134(3) 1_655 ? 
O2 K1 2.746(3) . ? 
C7 C8 1.4200 . ? 
C7 C11 1.4200 . ? 
C7 H7A 0.9800 . ? 
C8 C9 1.4200 . ? 
C8 H8A 0.9800 . ? 
C9 C10 1.4200 . ? 
C9 H9A 0.9800 . ? 
C10 C11 1.4200 . ? 
C10 H10A 0.9800 . ? 
C11 C12 1.498(4) . ? 
C12 O4 1.228(4) . ? 
C12 O3 1.281(5) . ? 
O3 K1 3.188(3) 1_655 ? 
O3 H300 1.0203 . ? 
O4 K1 2.938(3) . ? 
K1 O2 2.746(3) 2_557 ? 
K1 O4 2.938(3) 2_557 ? 
K1 O1 3.134(3) 1_455 ? 
K1 O1 3.134(3) 2_657 ? 
K1 O3 3.188(3) 1_455 ? 
K1 O3 3.188(3) 2_657 ? 

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 
C8 Co1 C1 121.74(9) . . ? 
C8 Co1 C9 41.0 . . ? 
C1 Co1 C9 157.82(10) . . ? 
C8 Co1 C5 159.47(10) . . ? 
C1 Co1 C5 41.0 . . ? 
C9 Co1 C5 159.02(10) . . ? 
C8 Co1 C7 40.9 . . ? 
C1 Co1 C7 107.01(9) . . ? 
C9 Co1 C7 68.89(6) . . ? 
C5 Co1 C7 124.19(9) . . ? 
C8 Co1 C2 104.96(9) . . ? 
C1 Co1 C2 40.9 . . ? 
C9 Co1 C2 121.10(9) . . ? 
C5 Co1 C2 68.84(6) . . ? 
C7 Co1 C2 120.87(9) . . ? 
C8 Co1 C10 68.87(6) . . ? 
C1 Co1 C10 159.83(10) . . ? 
C9 Co1 C10 40.9 . . ? 
C5 Co1 C10 123.93(9) . . ? 
C7 Co1 C10 68.8 . . ? 
C2 Co1 C10 158.42(10) . . ? 
C8 Co1 C11 68.85(6) . . ? 
C1 Co1 C11 123.23(9) . . ? 
C9 Co1 C11 68.82(5) . . ? 
C5 Co1 C11 109.21(8) . . ? 
C7 Co1 C11 40.9 . . ? 
C2 Co1 C11 158.07(10) . . ? 
C10 Co1 C11 40.8 . . ? 
C8 Co1 C4 156.90(10) . . ? 
C1 Co1 C4 68.84(5) . . ? 
C9 Co1 C4 121.94(9) . . ? 
C5 Co1 C4 40.9 . . ? 
C7 Co1 C4 161.33(10) . . ? 
C2 Co1 C4 68.69(6) . . ? 
C10 Co1 C4 108.45(9) . . ? 
C11 Co1 C4 125.07(9) . . ? 
C8 Co1 C3 120.10(9) . . ? 
C1 Co1 C3 68.75(6) . . ? 
C9 Co1 C3 105.82(9) . . ? 
C5 Co1 C3 68.75(6) . . ? 
C7 Co1 C3 156.41(10) . . ? 
C2 Co1 C3 40.8 . . ? 
C10 Co1 C3 123.11(9) . . ? 
C11 Co1 C3 160.59(10) . . ? 
C4 Co1 C3 40.8 . . ? 
C2 C1 C5 108.0 . . ? 
C2 C1 Co1 69.84(9) . . ? 
C5 C1 Co1 69.52(9) . . ? 
C2 C1 H1A 126.0 . . ? 
C5 C1 H1A 126.0 . . ? 
Co1 C1 H1A 126.0 . . ? 
C3 C2 C1 108.0 . . ? 
C3 C2 Co1 69.79(9) . . ? 
C1 C2 Co1 69.27(9) . . ? 
C3 C2 H2A 126.0 . . ? 
C1 C2 H2A 126.0 . . ? 
Co1 C2 H2A 126.0 . . ? 
C2 C3 C4 108.0 . . ? 
C2 C3 Co1 69.44(9) . . ? 
C4 C3 Co1 69.44(9) . . ? 
C2 C3 H3A 126.0 . . ? 
C4 C3 H3A 126.0 . . ? 
Co1 C3 H3A 126.0 . . ? 
C5 C4 C3 108.0 . . ? 
C5 C4 Co1 69.27(9) . . ? 
C3 C4 Co1 69.79(9) . . ? 
C5 C4 H4A 126.0 . . ? 
C3 C4 H4A 126.0 . . ? 
Co1 C4 H4A 126.0 . . ? 
C4 C5 C1 108.0 . . ? 
C4 C5 C6 127.7(2) . . ? 
C1 C5 C6 124.3(2) . . ? 
C4 C5 Co1 69.84(9) . . ? 
C1 C5 Co1 69.51(9) . . ? 
C6 C5 Co1 124.15(18) . . ? 
O2 C6 O1 126.5(3) . . ? 
O2 C6 C5 119.2(3) . . ? 
O1 C6 C5 114.4(3) . . ? 
C6 O1 K1 140.9(2) . 1_655 ? 
C6 O2 K1 129.3(2) . . ? 
C8 C7 C11 108.0 . . ? 
C8 C7 Co1 69.40(9) . . ? 
C11 C7 Co1 69.72(9) . . ? 
C8 C7 H7A 126.0 . . ? 
C11 C7 H7A 126.0 . . ? 
Co1 C7 H7A 126.0 . . ? 
C7 C8 C9 108.0 . . ? 
C7 C8 Co1 69.65(9) . . ? 
C9 C8 Co1 69.60(9) . . ? 
C7 C8 H8A 126.0 . . ? 
C9 C8 H8A 126.0 . . ? 
Co1 C8 H8A 126.0 . . ? 
C10 C9 C8 108.0 . . ? 
C10 C9 Co1 69.73(9) . . ? 
C8 C9 Co1 69.44(9) . . ? 
C10 C9 H9A 126.0 . . ? 
C8 C9 H9A 126.0 . . ? 
Co1 C9 H9A 126.0 . . ? 
C11 C10 C9 108.0 . . ? 
C11 C10 Co1 69.61(9) . . ? 
C9 C10 Co1 69.38(9) . . ? 
C11 C10 H10A 126.0 . . ? 
C9 C10 H10A 126.0 . . ? 
Co1 C10 H10A 126.0 . . ? 
C10 C11 C7 108.0 . . ? 
C10 C11 C12 127.2(2) . . ? 
C7 C11 C12 124.6(2) . . ? 
C10 C11 Co1 69.55(9) . . ? 
C7 C11 Co1 69.41(9) . . ? 
C12 C11 Co1 123.18(19) . . ? 
O4 C12 O3 126.2(3) . . ? 
O4 C12 C11 119.5(3) . . ? 
O3 C12 C11 114.3(3) . . ? 
C12 O3 K1 143.4(2) . 1_655 ? 
C12 O3 H300 108.0 . . ? 
K1 O3 H300 91.6 1_655 . ? 
C12 O4 K1 123.5(3) . . ? 
O2 K1 O2 180.00(11) 2_557 . ? 
O2 K1 O4 67.26(8) 2_557 2_557 ? 
O2 K1 O4 112.74(8) . 2_557 ? 
O2 K1 O4 112.74(8) 2_557 . ? 
O2 K1 O4 67.26(8) . . ? 
O4 K1 O4 180.0 2_557 . ? 
O2 K1 O1 95.37(7) 2_557 1_455 ? 
O2 K1 O1 84.63(7) . 1_455 ? 
O4 K1 O1 63.43(8) 2_557 1_455 ? 
O4 K1 O1 116.57(8) . 1_455 ? 
O2 K1 O1 84.63(7) 2_557 2_657 ? 
O2 K1 O1 95.37(7) . 2_657 ? 
O4 K1 O1 116.57(8) 2_557 2_657 ? 
O4 K1 O1 63.43(8) . 2_657 ? 
O1 K1 O1 180.00(6) 1_455 2_657 ? 
O2 K1 O3 64.39(8) 2_557 1_455 ? 
O2 K1 O3 115.61(8) . 1_455 ? 
O4 K1 O3 99.33(7) 2_557 1_455 ? 
O4 K1 O3 80.67(7) . 1_455 ? 
O1 K1 O3 61.74(7) 1_455 1_455 ? 
O1 K1 O3 118.26(7) 2_657 1_455 ? 
O2 K1 O3 115.61(8) 2_557 2_657 ? 
O2 K1 O3 64.39(8) . 2_657 ? 
O4 K1 O3 80.67(7) 2_557 2_657 ? 
O4 K1 O3 99.33(7) . 2_657 ? 
O1 K1 O3 118.26(7) 1_455 2_657 ? 
O1 K1 O3 61.74(7) 2_657 2_657 ? 
O3 K1 O3 180.0 1_455 2_657 ? 

_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              24.97 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    0.438 
_refine_diff_density_min   -0.607 
_refine_diff_density_rms    0.082