# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Jose Martinez-Lillo'
_publ_contact_author_email       LILLO@UV.ES

_publ_section_title              
;
A Self-assembled Tetrameric Water Cluster stabilized
by the Hexachlororhenate(IV) Anion and diprotonated 2,2'-Biimidazole :
X-ray Structure and Magnetic Properties
;
loop_
_publ_author_name
"Jos\'e Martinez-Lillo"
'Donatella Armentano'
'G.De Munno'
'Juan Faus'
'Miguel Julve'
;
F.Lloret
;
'Nadia Marino'

# Attachment 'Compound1.CIF'

data_1
_database_code_depnum_ccdc_archive 'CCDC 685653'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H8 Cl3 N2 O2 Re0.50'
_chemical_formula_weight         303.56

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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                   7.9626(10)
_cell_length_b                   8.0241(10)
_cell_length_c                   8.1598(10)
_cell_angle_alpha                108.788(3)
_cell_angle_beta                 111.666(2)
_cell_angle_gamma                99.606(3)
_cell_volume                     433.83(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8024
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      35.10

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            pale-green-yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             289
_exptl_absorpt_coefficient_mu    7.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_T_max  0.388
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'X8APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6565
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         28.28
_reflns_number_total             2153
_reflns_number_gt                2153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0138P)^2^+0.1396P] 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         2153
_refine_ls_number_parameters     109
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0122
_refine_ls_wR_factor_ref         0.0312
_refine_ls_wR_factor_gt          0.0312
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.120
_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
N1 N 0.1801(2) 0.9024(2) 0.9497(2) 0.0116(3) Uani 1 1 d . . .
H1 H 0.2140 0.9533 0.8839 0.014 Uiso 1 1 calc R . .
N2 N 0.0371(2) 0.8300(2) 1.1083(2) 0.0111(3) Uani 1 1 d . . .
H2 H -0.0377 0.8255 1.1617 0.013 Uiso 1 1 calc R . .
C1 C 0.2495(3) 0.7742(3) 1.0065(3) 0.0144(4) Uani 1 1 d . . .
H1A H 0.3403 0.7269 0.9806 0.017 Uiso 1 1 calc R . .
C2 C 0.1612(3) 0.7297(3) 1.1071(3) 0.0136(4) Uani 1 1 d . . .
H2A H 0.1806 0.6470 1.1645 0.016 Uiso 1 1 calc R . .
C3 C 0.0513(3) 0.9354(3) 1.0134(3) 0.0097(3) Uani 1 1 d . . .
O1W O 0.1372(2) 1.2548(2) 0.6816(2) 0.0198(3) Uani 1 1 d D . .
O2W O 0.2379(2) 0.9419(2) 0.6558(2) 0.0194(3) Uani 1 1 d D . .
H1W H 0.032(3) 1.241(4) 0.571(3) 0.050 Uiso 1 1 d D . .
H2W H 0.230(3) 1.365(3) 0.715(4) 0.050 Uiso 1 1 d D . .
H3W H 0.246(5) 1.055(3) 0.644(5) 0.050 Uiso 1 1 d D . .
H4W H 0.335(4) 0.906(4) 0.630(5) 0.050 Uiso 1 1 d D . .
Re1 Re 0.5000 1.5000 0.5000 0.00662(4) Uani 1 2 d S . .
Cl1 Cl 0.43065(6) 1.18436(6) 0.44502(7) 0.01180(9) Uani 1 1 d . . .
Cl2 Cl 0.44027(6) 1.42015(7) 0.17285(6) 0.01248(9) Uani 1 1 d . . .
Cl3 Cl 0.17759(6) 1.47562(6) 0.41337(7) 0.01169(9) 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
N1 0.0106(7) 0.0128(8) 0.0121(8) 0.0052(7) 0.0059(6) 0.0036(6)
N2 0.0098(7) 0.0122(8) 0.0110(7) 0.0052(6) 0.0043(6) 0.0034(6)
C1 0.0110(8) 0.0141(10) 0.0159(9) 0.0046(8) 0.0048(7) 0.0054(7)
C2 0.0118(8) 0.0116(9) 0.0140(9) 0.0048(8) 0.0027(7) 0.0042(7)
C3 0.0084(8) 0.0106(9) 0.0073(8) 0.0026(7) 0.0021(7) 0.0016(7)
O1W 0.0250(8) 0.0209(8) 0.0241(8) 0.0143(7) 0.0165(7) 0.0096(7)
O2W 0.0255(8) 0.0212(8) 0.0242(8) 0.0138(7) 0.0179(7) 0.0135(7)
Re1 0.00599(5) 0.00732(6) 0.00689(6) 0.00295(4) 0.00315(4) 0.00244(4)
Cl1 0.01242(19) 0.0089(2) 0.0142(2) 0.00491(17) 0.00619(17) 0.00330(16)
Cl2 0.0128(2) 0.0163(2) 0.0089(2) 0.00498(18) 0.00553(17) 0.00512(17)
Cl3 0.00775(18) 0.0144(2) 0.0144(2) 0.00725(18) 0.00516(16) 0.00441(16)

_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
N1 C3 1.337(2) . ?
N1 C1 1.373(2) . ?
N1 H1 0.8600 . ?
N2 C3 1.335(2) . ?
N2 C2 1.375(2) . ?
N2 H2 0.8600 . ?
C1 C2 1.352(3) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C3 1.445(3) 2_577 ?
O1W H1W 0.937(10) . ?
O1W H2W 0.938(10) . ?
O2W H3W 0.942(10) . ?
O2W H4W 0.941(10) . ?
Re1 Cl3 2.3520(5) 2_686 ?
Re1 Cl3 2.3520(5) . ?
Re1 Cl1 2.3536(5) 2_686 ?
Re1 Cl1 2.3536(5) . ?
Re1 Cl2 2.3711(5) . ?
Re1 Cl2 2.3711(5) 2_686 ?

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
C3 N1 C1 108.93(16) . . ?
C3 N1 H1 125.5 . . ?
C1 N1 H1 125.5 . . ?
C3 N2 C2 109.09(16) . . ?
C3 N2 H2 125.5 . . ?
C2 N2 H2 125.5 . . ?
C2 C1 N1 107.24(17) . . ?
C2 C1 H1A 126.4 . . ?
N1 C1 H1A 126.4 . . ?
C1 C2 N2 106.92(17) . . ?
C1 C2 H2A 126.5 . . ?
N2 C2 H2A 126.5 . . ?
N2 C3 N1 107.81(15) . . ?
N2 C3 C3 126.3(2) . 2_577 ?
N1 C3 C3 125.8(2) . 2_577 ?
H1W O1W H2W 105.3(14) . . ?
H3W O2W H4W 104.4(14) . . ?
Cl3 Re1 Cl3 180.000(6) 2_686 . ?
Cl3 Re1 Cl1 90.486(16) 2_686 2_686 ?
Cl3 Re1 Cl1 89.514(16) . 2_686 ?
Cl3 Re1 Cl1 89.514(16) 2_686 . ?
Cl3 Re1 Cl1 90.486(16) . . ?
Cl1 Re1 Cl1 180.0 2_686 . ?
Cl3 Re1 Cl2 89.743(15) 2_686 . ?
Cl3 Re1 Cl2 90.257(15) . . ?
Cl1 Re1 Cl2 89.279(16) 2_686 . ?
Cl1 Re1 Cl2 90.721(16) . . ?
Cl3 Re1 Cl2 90.257(15) 2_686 2_686 ?
Cl3 Re1 Cl2 89.743(15) . 2_686 ?
Cl1 Re1 Cl2 90.721(16) 2_686 2_686 ?
Cl1 Re1 Cl2 89.279(16) . 2_686 ?
Cl2 Re1 Cl2 180.0 . 2_686 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O2W 0.86 1.91 2.706(2) 152.2 .
N2 H2 O1W 0.86 1.95 2.742(2) 153.4 2_577
O1W H1W O2W 0.937(10) 2.109(18) 2.923(2) 144(2) 2_576
O2W H3W O1W 0.942(10) 1.937(19) 2.729(2) 140(3) .
O1W H2W Cl2 0.938(10) 2.531(14) 3.4145(18) 157(3) 2_686
O2W H3W Cl1 0.942(10) 2.86(3) 3.4936(16) 126(2) .
O2W H4W Cl1 0.941(10) 2.319(10) 3.2600(16) 178(3) 2_676

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.103