# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Biserka Kojic-Prodic'
_publ_contact_author_email       KOJIC@IRB.HR

_publ_section_title              
;
pi-Stacking of quinoid rings
in crystals of alkali diaqua hydrogen chloranilates
;
loop_
_publ_author_name
'Biserka Kojic-Prodic'
'Anton Meden'
'Kresimir Molcanov'

data_CsHCA(H2O)2
_database_code_depnum_ccdc_archive 'CCDC 669451'

_audit_creation_date             2007-08-22T16:38:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C6 H5 Cl2 Cs1 O6'
_chemical_formula_sum            'C6 H5 Cl2 Cs O6'
_chemical_formula_weight         376.91

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
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                   9.3968(2)
_cell_length_b                   7.07250(10)
_cell_length_c                   15.8292(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.3770(10)
_cell_angle_gamma                90
_cell_volume                     1048.92(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2556
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
based on the redundancy of symmetry-related
measurements
;
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_T_max  0.980
_exptl_special_details           
;
KappaCCD Nonius diffractometer.
214 frames in 7 sets of ω and φ scans at κ = 55°. Rotation/frame=2°.
Crystal-detector distance=35.0 mm. Measuring time=100 s/frame.
Mosaicity=0.407(2)°.
;

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       
;
ω scans at κ=55°
;
_diffrn_detector_area_resol_mean 0.055
_diffrn_reflns_number            4532
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_reflns_number_total             2398
_reflns_number_gt                2082
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.0209P)²+0.9535P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0119(5)
_refine_ls_number_reflns         2398
_refine_ls_number_parameters     153
_refine_ls_number_restraints     6
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0568
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.05
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.929

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.368 2.119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
O6 O 0.8735(3) 0.9506(4) 0.20917(14) 0.0552(7) Uani 1 d D . .
O5 O 1.0280(3) 0.1243(5) 0.08548(17) 0.0656(7) Uani 1 d D . .
O4 O 0.6617(2) 0.3924(3) 0.11936(11) 0.0400(5) Uani 1 d . . .
H6A H 0.891(5) 0.958(6) 0.2683(7) 0.082(14) Uiso 1 d D . .
H6B H 0.941(4) 1.028(6) 0.186(3) 0.11(2) Uiso 1 d D . .
H5B H 1.109(4) 0.141(9) 0.056(3) 0.14(2) Uiso 1 d D . .
H5A H 0.950(4) 0.120(9) 0.046(3) 0.13(2) Uiso 1 d D . .
Cs1 Cs 0.961037(18) 0.54890(3) 0.146491(11) 0.04292(10) Uani 1 d . . .
Cl2 Cl 0.36285(7) 0.26700(11) 0.14122(4) 0.03605(17) Uani 1 d . . .
Cl1 Cl 0.68969(8) 0.23323(12) -0.19311(4) 0.0440(2) Uani 1 d . . .
C6 C 0.5959(3) 0.3237(4) 0.05552(15) 0.0269(5) Uani 1 d . . .
O3 O 0.25617(19) 0.1355(3) -0.03168(11) 0.0377(5) Uani 1 d . . .
O2 O 0.3939(2) 0.1237(3) -0.17297(11) 0.0368(4) Uani 1 d . . .
H H 0.312 0.0955 -0.1633 0.055 Uiso 1 calc R . .
O1 O 0.80277(19) 0.3564(3) -0.02160(12) 0.0408(5) Uani 1 d . . .
C2 C 0.6008(3) 0.2413(4) -0.10172(14) 0.0273(5) Uani 1 d . . .
C3 C 0.4631(3) 0.1857(4) -0.10277(15) 0.0262(5) Uani 1 d . . .
C4 C 0.3821(3) 0.1913(4) -0.02393(15) 0.0255(5) Uani 1 d . . .
C1 C 0.6776(3) 0.3097(4) -0.02537(15) 0.0281(5) Uani 1 d . . .
C5 C 0.4551(3) 0.2595(4) 0.05027(14) 0.0256(5) Uani 1 d . . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
O6 H6A 0.940(10) . ?
O6 H6B 0.938(10) . ?
O5 H5B 0.927(19) . ?
O5 H5A 0.931(19) . ?
O4 C6 1.242(3) . ?
Cl2 C5 1.737(2) . ?
Cl1 C2 1.726(2) . ?
C6 C5 1.395(3) . ?
C6 C1 1.545(3) . ?
O3 C4 1.244(3) . ?
O2 C3 1.319(3) . ?
O2 H 0.82 . ?
O1 C1 1.219(3) . ?
C2 C3 1.352(4) . ?
C2 C1 1.443(3) . ?
C3 C4 1.511(3) . ?
C4 C5 1.400(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
H6A O6 H6B 107(2) . . ?
H5B O5 H5A 107(3) . . ?
O4 C6 C5 125.9(2) . . ?
O4 C6 C1 116.8(2) . . ?
C5 C6 C1 117.3(2) . . ?
C3 O2 H 109.5 . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 Cl1 120.28(19) . . ?
C1 C2 Cl1 118.04(18) . . ?
O2 C3 C2 121.1(2) . . ?
O2 C3 C4 117.2(2) . . ?
C2 C3 C4 121.6(2) . . ?
O3 C4 C5 126.4(2) . . ?
O3 C4 C3 116.5(2) . . ?
C5 C4 C3 117.1(2) . . ?
O1 C1 C2 123.4(2) . . ?
O1 C1 C6 118.7(2) . . ?
C2 C1 C6 117.9(2) . . ?
C6 C5 C4 124.3(2) . . ?
C6 C5 Cl2 118.13(18) . . ?
C4 C5 Cl2 117.53(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 O2 179.9(2) . . . . ?
Cl1 C2 C3 O2 0.3(4) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
Cl1 C2 C3 C4 -179.92(19) . . . . ?
O2 C3 C4 O3 0.4(4) . . . . ?
C2 C3 C4 O3 -179.4(3) . . . . ?
O2 C3 C4 C5 -179.2(2) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
C3 C2 C1 O1 178.0(3) . . . . ?
Cl1 C2 C1 O1 -2.3(4) . . . . ?
C3 C2 C1 C6 -1.9(4) . . . . ?
Cl1 C2 C1 C6 177.77(19) . . . . ?
O4 C6 C1 O1 3.8(4) . . . . ?
C5 C6 C1 O1 -176.6(3) . . . . ?
O4 C6 C1 C2 -176.3(3) . . . . ?
C5 C6 C1 C2 3.4(4) . . . . ?
O4 C6 C5 C4 176.8(3) . . . . ?
C1 C6 C5 C4 -2.8(4) . . . . ?
O4 C6 C5 Cl2 -2.4(4) . . . . ?
C1 C6 C5 Cl2 178.05(18) . . . . ?
O3 C4 C5 C6 -178.8(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
O3 C4 C5 Cl2 0.3(4) . . . . ?
C3 C4 C5 Cl2 179.85(18) . . . . ?

data_KHCA(H2O)2
_database_code_depnum_ccdc_archive 'CCDC 669452'

_audit_creation_date             2007-09-13T11:37:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C6 H5 Cl2 K1 O6'
_chemical_formula_sum            'C6 H5 Cl2 K1 O6'
_chemical_formula_weight         283.11

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
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                   10.0492(8)
_cell_length_b                   15.2833(14)
_cell_length_c                   6.4546(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.156(9)
_cell_angle_gamma                90
_cell_volume                     978.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28
_cell_measurement_theta_min      9.3
_cell_measurement_theta_max      22

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            'dark purple'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             568
_exptl_absorpt_coefficient_mu    9.91
_exptl_absorpt_correction_type   none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        1
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 0 1
-1 -2 -3
-1 -4 2

_diffrn_reflns_number            2219
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         4.46
_diffrn_reflns_theta_max         76.27
_diffrn_reflns_theta_full        76.27
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_reflns_number_total             2034
_reflns_number_gt                1678
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.0704P)²+0.2340P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0034(5)
_refine_ls_number_reflns         2034
_refine_ls_number_parameters     157
_refine_ls_number_restraints     6
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1144
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.492

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.364 0.702 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.387 1.066 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.049 0.032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
K1 K 0.18680(6) 0.94066(4) 0.15721(10) 0.0351(2) Uani 1 d . . .
O5 O 0.3705(3) 0.91558(14) 0.5328(4) 0.0416(5) Uani 1 d D . .
O6 O 0.2892(2) 0.82838(16) -0.1284(4) 0.0413(5) Uani 1 d D . .
Cl2 Cl 0.00111(7) 0.59205(4) 0.15464(11) 0.0301(2) Uani 1 d . . .
Cl1 Cl -0.40254(7) 0.91263(4) 0.06786(12) 0.0336(2) Uani 1 d . . .
O1 O -0.10371(19) 0.91727(11) 0.1172(3) 0.0301(4) Uani 1 d . . .
O2 O -0.46913(19) 0.72340(13) 0.0515(3) 0.0315(5) Uani 1 d . . .
O3 O -0.29981(19) 0.59104(12) 0.0968(3) 0.0304(5) Uani 1 d . . .
O4 O 0.07166(19) 0.78313(12) 0.1886(3) 0.0311(5) Uani 1 d . . .
C6 C -0.0502(3) 0.76556(16) 0.1519(4) 0.0226(5) Uani 1 d . . .
C4 C -0.2449(3) 0.66445(16) 0.1033(4) 0.0222(5) Uani 1 d . . .
C2 C -0.2928(2) 0.82509(16) 0.0919(4) 0.0233(5) Uani 1 d . . .
C3 C -0.3390(3) 0.74180(17) 0.0814(4) 0.0226(5) Uani 1 d . . .
C1 C -0.1492(2) 0.84347(16) 0.1206(4) 0.0221(5) Uani 1 d . . .
C5 C -0.1066(2) 0.68069(15) 0.1333(4) 0.0232(5) Uani 1 d . . .
H6A H 0.212(3) 0.793(3) -0.150(9) 0.12(2) Uiso 1 d D . .
H6B H 0.359(3) 0.791(3) -0.072(8) 0.102(19) Uiso 1 d D . .
H H -0.485(4) 0.673(3) 0.042(7) 0.062(13) Uiso 1 d . . .
H5A H 0.343(6) 0.893(3) 0.655(6) 0.12(2) Uiso 1 d D . .
H5B H 0.385(5) 0.9740(15) 0.567(8) 0.105(19) Uiso 1 d D . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
K1 O4 2.693(2) . ?
K1 O6 2.830(2) . ?
K1 O5 2.830(3) . ?
K1 O1 2.8422(19) 3_575 ?
K1 O1 2.912(2) . ?
K1 O3 2.919(2) 2 ?
K1 Cl2 3.3353(10) 2 ?
K1 Cl2 3.5111(11) 4_575 ?
K1 C6 3.579(3) . ?
K1 Cl1 3.5834(10) 3_575 ?
K1 K1 4.3679(13) 3_575 ?
K1 H6A 3.04(5) . ?
K1 H5B 3.09(5) . ?
O5 H5A 0.940(19) . ?
O5 H5B 0.926(19) . ?
O6 H6A 0.937(19) . ?
O6 H6B 0.932(19) . ?
Cl2 C5 1.726(2) . ?
Cl2 K1 3.3353(10) 2_545 ?
Cl2 K1 3.5111(11) 4_576 ?
Cl1 C2 1.725(2) . ?
Cl1 K1 3.5834(10) 3_575 ?
O1 C1 1.219(3) . ?
O1 K1 2.8422(19) 3_575 ?
O2 C3 1.321(3) . ?
O2 H 0.78(4) . ?
O3 C4 1.248(3) . ?
O3 K1 2.919(2) 2_545 ?
O4 C6 1.239(3) . ?
C6 C5 1.413(3) . ?
C6 C1 1.545(3) . ?
C4 C5 1.395(3) . ?
C4 C3 1.506(3) . ?
C2 C3 1.353(4) . ?
C2 C1 1.453(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
O4 K1 O6 73.26(7) . . ?
O4 K1 O5 92.53(7) . . ?
O6 K1 O5 102.74(7) . . ?
O4 K1 O1 130.00(6) . 3_575 ?
O6 K1 O1 99.13(7) . 3_575 ?
O5 K1 O1 136.41(6) . 3_575 ?
O4 K1 O1 57.32(5) . . ?
O6 K1 O1 109.35(6) . . ?
O5 K1 O1 124.58(7) . . ?
O1 K1 O1 81.23(6) 3_575 . ?
O4 K1 O3 142.92(6) . 2 ?
O6 K1 O3 132.96(6) . 2 ?
O5 K1 O3 59.76(6) . 2 ?
O1 K1 O3 77.74(6) 3_575 2 ?
O1 K1 O3 116.28(6) . 2 ?
O4 K1 Cl2 108.54(5) . 2 ?
O6 K1 Cl2 160.68(5) . 2 ?
O5 K1 Cl2 96.43(5) . 2 ?
O1 K1 Cl2 64.52(4) 3_575 2 ?
O1 K1 Cl2 59.98(4) . 2 ?
O3 K1 Cl2 56.60(4) 2 2 ?
O4 K1 Cl2 76.74(5) . 4_575 ?
O6 K1 Cl2 60.45(5) . 4_575 ?
O5 K1 Cl2 161.90(5) . 4_575 ?
O1 K1 Cl2 58.19(4) 3_575 4_575 ?
O1 K1 Cl2 61.48(4) . 4_575 ?
O3 K1 Cl2 135.91(4) 2 4_575 ?
Cl2 K1 Cl2 100.76(2) 2 4_575 ?
O4 K1 C6 16.03(6) . . ?
O6 K1 C6 81.41(6) . . ?
O5 K1 C6 104.44(7) . . ?
O1 K1 C6 115.87(6) 3_575 . ?
O1 K1 C6 41.50(5) . . ?
O3 K1 C6 142.64(6) 2 . ?
Cl2 K1 C6 96.19(4) 2 . ?
Cl2 K1 C6 68.26(4) 4_575 . ?
O4 K1 Cl1 152.23(5) . 3_575 ?
O6 K1 Cl1 78.99(5) . 3_575 ?
O5 K1 Cl1 94.46(6) . 3_575 ?
O1 K1 Cl1 53.56(4) 3_575 3_575 ?
O1 K1 Cl1 134.72(4) . 3_575 ?
O3 K1 Cl1 61.29(4) 2 3_575 ?
Cl2 K1 Cl1 97.33(2) 2 3_575 ?
Cl2 K1 Cl1 88.94(2) 4_575 3_575 ?
C6 K1 Cl1 155.31(5) . 3_575 ?
O4 K1 K1 93.35(5) . 3_575 ?
O6 K1 K1 108.91(5) . 3_575 ?
O5 K1 K1 148.17(6) . 3_575 ?
O1 K1 K1 41.21(4) 3_575 3_575 ?
O1 K1 K1 40.02(4) . 3_575 ?
O3 K1 K1 99.04(4) 2 3_575 ?
Cl2 K1 K1 52.158(19) 2 3_575 ?
Cl2 K1 K1 48.604(18) 4_575 3_575 ?
C6 K1 K1 77.56(4) . 3_575 ?
Cl1 K1 K1 94.74(2) 3_575 3_575 ?
O4 K1 H6A 57.8(8) . . ?
O6 K1 H6A 17.9(5) . . ?
O5 K1 H6A 110.2(9) . . ?
O1 K1 H6A 102.0(10) 3_575 . ?
O1 K1 H6A 92.2(5) . . ?
O3 K1 H6A 150.8(5) 2 . ?
Cl2 K1 H6A 149.7(7) 2 . ?
Cl2 K1 H6A 51.7(9) 4_575 . ?
C6 K1 H6A 64.1(6) . . ?
Cl1 K1 H6A 94.7(7) 3_575 . ?
K1 K1 H6A 99.3(8) 3_575 . ?
O4 K1 H5B 108.1(6) . . ?
O6 K1 H5B 113.9(8) . . ?
O5 K1 H5B 17.3(5) . . ?
O1 K1 H5B 119.5(5) 3_575 . ?
O1 K1 H5B 126.7(9) . . ?
O3 K1 H5B 42.5(5) 2 . ?
Cl2 K1 H5B 84.2(8) 2 . ?
Cl2 K1 H5B 171.8(9) 4_575 . ?
C6 K1 H5B 118.0(7) . . ?
Cl1 K1 H5B 83.9(8) 3_575 . ?
K1 K1 H5B 136.0(7) 3_575 . ?
H6A K1 H5B 124.7(11) . . ?
K1 O5 H5A 122(4) . . ?
K1 O5 H5B 97(3) . . ?
H5A O5 H5B 103(3) . . ?
K1 O6 H6A 94(4) . . ?
K1 O6 H6B 117(3) . . ?
H6A O6 H6B 105(3) . . ?
C5 Cl2 K1 100.90(9) . 2_545 ?
C5 Cl2 K1 114.82(9) . 4_576 ?
K1 Cl2 K1 79.24(2) 2_545 4_576 ?
C2 Cl1 K1 95.89(9) . 3_575 ?
C1 O1 K1 130.12(17) . 3_575 ?
C1 O1 K1 119.07(16) . . ?
K1 O1 K1 98.77(6) 3_575 . ?
C3 O2 H 114(3) . . ?
C4 O3 K1 123.92(16) . 2_545 ?
C6 O4 K1 127.07(16) . . ?
O4 C6 C5 125.9(2) . . ?
O4 C6 C1 117.0(2) . . ?
C5 C6 C1 117.0(2) . . ?
O4 C6 K1 36.89(12) . . ?
C5 C6 K1 160.88(17) . . ?
C1 C6 K1 80.72(13) . . ?
O3 C4 C5 126.1(2) . . ?
O3 C4 C3 115.8(2) . . ?
C5 C4 C3 118.0(2) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 Cl1 121.1(2) . . ?
C1 C2 Cl1 117.98(19) . . ?
O2 C3 C2 122.1(2) . . ?
O2 C3 C4 116.0(2) . . ?
C2 C3 C4 121.9(2) . . ?
O1 C1 C2 123.0(2) . . ?
O1 C1 C6 118.7(2) . . ?
C2 C1 C6 118.3(2) . . ?
C4 C5 C6 123.6(2) . . ?
C4 C5 Cl2 118.04(18) . . ?
C6 C5 Cl2 118.37(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 K1 O1 C1 -4.36(18) . . . . ?
O6 K1 O1 C1 49.6(2) . . . . ?
O5 K1 O1 C1 -72.1(2) . . . . ?
O1 K1 O1 C1 146.3(2) 3_575 . . . ?
O3 K1 O1 C1 -142.13(18) 2 . . . ?
Cl2 K1 O1 C1 -148.2(2) 2 . . . ?
Cl2 K1 O1 C1 87.83(19) 4_575 . . . ?
C6 K1 O1 C1 -0.91(17) . . . . ?
Cl1 K1 O1 C1 143.23(17) 3_575 . . . ?
K1 K1 O1 C1 146.3(2) 3_575 . . . ?
O4 K1 O1 K1 -150.64(9) . . . 3_575 ?
O6 K1 O1 K1 -96.66(7) . . . 3_575 ?
O5 K1 O1 K1 141.60(7) . . . 3_575 ?
O1 K1 O1 K1 0 3_575 . . 3_575 ?
O3 K1 O1 K1 71.59(8) 2 . . 3_575 ?
Cl2 K1 O1 K1 65.56(4) 2 . . 3_575 ?
Cl2 K1 O1 K1 -58.45(4) 4_575 . . 3_575 ?
C6 K1 O1 K1 -147.19(11) . . . 3_575 ?
Cl1 K1 O1 K1 -3.05(8) 3_575 . . 3_575 ?
O6 K1 O4 C6 -118.8(2) . . . . ?
O5 K1 O4 C6 138.6(2) . . . . ?
O1 K1 O4 C6 -30.9(2) 3_575 . . . ?
O1 K1 O4 C6 8.3(2) . . . . ?
O3 K1 O4 C6 99.7(2) 2 . . . ?
Cl2 K1 O4 C6 41.0(2) 2 . . . ?
Cl2 K1 O4 C6 -56.1(2) 4_575 . . . ?
Cl1 K1 O4 C6 -116.9(2) 3_575 . . . ?
K1 K1 O4 C6 -10.1(2) 3_575 . . . ?
K1 O4 C6 C5 168.08(19) . . . . ?
K1 O4 C6 C1 -11.0(3) . . . . ?
O6 K1 C6 O4 58.0(2) . . . . ?
O5 K1 C6 O4 -43.0(2) . . . . ?
O1 K1 C6 O4 154.1(2) 3_575 . . . ?
O1 K1 C6 O4 -169.4(3) . . . . ?
O3 K1 C6 O4 -101.7(2) 2 . . . ?
Cl2 K1 C6 O4 -141.3(2) 2 . . . ?
Cl2 K1 C6 O4 119.6(2) 4_575 . . . ?
Cl1 K1 C6 O4 95.8(2) 3_575 . . . ?
K1 K1 C6 O4 169.7(2) 3_575 . . . ?
O4 K1 C6 C5 -30.7(5) . . . . ?
O6 K1 C6 C5 27.3(5) . . . . ?
O5 K1 C6 C5 -73.7(5) . . . . ?
O1 K1 C6 C5 123.3(5) 3_575 . . . ?
O1 K1 C6 C5 159.9(6) . . . . ?
O3 K1 C6 C5 -132.4(5) 2 . . . ?
Cl2 K1 C6 C5 -172.0(5) 2 . . . ?
Cl2 K1 C6 C5 88.8(5) 4_575 . . . ?
Cl1 K1 C6 C5 65.1(6) 3_575 . . . ?
K1 K1 C6 C5 139.0(5) 3_575 . . . ?
O4 K1 C6 C1 170.0(3) . . . . ?
O6 K1 C6 C1 -131.92(14) . . . . ?
O5 K1 C6 C1 127.04(13) . . . . ?
O1 K1 C6 C1 -35.89(15) 3_575 . . . ?
O1 K1 C6 C1 0.63(12) . . . . ?
O3 K1 C6 C1 68.36(17) 2 . . . ?
Cl2 K1 C6 C1 28.74(13) 2 . . . ?
Cl2 K1 C6 C1 -70.40(13) 4_575 . . . ?
Cl1 K1 C6 C1 -94.18(16) 3_575 . . . ?
K1 K1 C6 C1 -20.27(12) 3_575 . . . ?
K1 O3 C4 C5 33.7(4) 2_545 . . . ?
K1 O3 C4 C3 -144.79(17) 2_545 . . . ?
K1 Cl1 C2 C3 -150.3(2) 3_575 . . . ?
K1 Cl1 C2 C1 28.7(2) 3_575 . . . ?
C1 C2 C3 O2 -178.7(2) . . . . ?
Cl1 C2 C3 O2 0.3(4) . . . . ?
C1 C2 C3 C4 1.4(4) . . . . ?
Cl1 C2 C3 C4 -179.61(19) . . . . ?
O3 C4 C3 O2 -1.9(3) . . . . ?
C5 C4 C3 O2 179.5(2) . . . . ?
O3 C4 C3 C2 178.0(2) . . . . ?
C5 C4 C3 C2 -0.6(4) . . . . ?
K1 O1 C1 C2 -42.9(4) 3_575 . . . ?
K1 O1 C1 C2 -177.03(18) . . . . ?
K1 O1 C1 C6 135.74(19) 3_575 . . . ?
K1 O1 C1 C6 1.6(3) . . . . ?
C3 C2 C1 O1 175.1(3) . . . . ?
Cl1 C2 C1 O1 -4.0(4) . . . . ?
C3 C2 C1 C6 -3.6(4) . . . . ?
Cl1 C2 C1 C6 177.39(18) . . . . ?
O4 C6 C1 O1 5.5(4) . . . . ?
C5 C6 C1 O1 -173.7(2) . . . . ?
K1 C6 C1 O1 -1.1(2) . . . . ?
O4 C6 C1 C2 -175.8(2) . . . . ?
C5 C6 C1 C2 5.0(3) . . . . ?
K1 C6 C1 C2 177.5(2) . . . . ?
O3 C4 C5 C6 -176.1(3) . . . . ?
C3 C4 C5 C6 2.4(4) . . . . ?
O3 C4 C5 Cl2 2.5(4) . . . . ?
C3 C4 C5 Cl2 -179.06(18) . . . . ?
O4 C6 C5 C4 176.3(3) . . . . ?
C1 C6 C5 C4 -4.6(4) . . . . ?
K1 C6 C5 C4 -161.4(4) . . . . ?
O4 C6 C5 Cl2 -2.2(4) . . . . ?
C1 C6 C5 Cl2 176.90(18) . . . . ?
K1 C6 C5 Cl2 20.0(7) . . . . ?
K1 Cl2 C5 C4 -27.1(2) 2_545 . . . ?
K1 Cl2 C5 C4 -110.2(2) 4_576 . . . ?
K1 Cl2 C5 C6 151.47(19) 2_545 . . . ?
K1 Cl2 C5 C6 68.4(2) 4_576 . . . ?

data_LiHCAEtOH
_database_code_depnum_ccdc_archive 'CCDC 669453'

_audit_creation_date             2007-09-12T15:48:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?
#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C8 H7 Cl2 Li O5'
_chemical_formula_sum            'C8 H7 Cl2 Li O5'
_chemical_formula_weight         260.98
_chemical_absolute_configuration unk

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.72(2)
_cell_length_b                   4.975(2)
_cell_length_c                   14.700(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1003.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      6.4
_cell_measurement_theta_max      19.1

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    5.873
_exptl_absorpt_correction_type   none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        2
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -4 0
2 -2 0
1 -3 2

_diffrn_reflns_number            1085
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         6.02
_diffrn_reflns_theta_max         76.21
_diffrn_reflns_theta_full        76.21
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_reflns_number_total             1085
_reflns_number_gt                960
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.1010P)²+0.2741P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1085
_refine_ls_number_parameters     171
_refine_ls_number_restraints     9
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1336
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.634

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
H7A H 0.209(6) 0.783(17) 0.303(5) 0.05(2) Uiso 1 d . . .
H7B H 0.231(4) 0.852(12) 0.400(4) 0.016(12) Uiso 1 d . . .
H8C H 0.168(5) 1.255(15) 0.284(2) 0.06 Uiso 1 d D . .
H8A H 0.0986(19) 1.146(11) 0.356(4) 0.038(16) Uiso 1 d D . .
H8B H 0.182(5) 1.343(10) 0.380(4) 0.06 Uiso 1 d D . .
H H 0.633(4) 0.707(8) -0.086(4) 0.037(17) Uiso 1 d D . .
H5 H 0.343(5) 1.136(11) 0.304(4) 0.05(2) Uiso 1 d D . .
Cl2 Cl 0.33685(9) 0.0578(2) 0.09206(9) 0.0329(4) Uani 1 d . . .
Cl1 Cl 0.66543(9) 0.9556(2) 0.08439(9) 0.0327(4) Uani 1 d . . .
O1 O 0.5263(3) 0.8236(9) 0.2334(4) 0.0334(11) Uani 1 d . . .
O2 O 0.6073(4) 0.5653(9) -0.0635(4) 0.0337(12) Uani 1 d D . .
O3 O 0.4775(3) 0.1953(8) -0.0565(4) 0.0323(11) Uani 1 d . . .
O4 O 0.3921(3) 0.4511(8) 0.2440(4) 0.0341(13) Uani 1 d . . .
O5 O 0.3321(2) 1.0197(6) 0.3427(5) 0.0307(7) Uani 1 d D . .
C2 C 0.5754(4) 0.7139(9) 0.0858(6) 0.0245(11) Uani 1 d . . .
C6 C 0.4373(4) 0.4649(10) 0.1701(5) 0.0236(13) Uani 1 d . . .
C7 C 0.2300(3) 0.9440(9) 0.3396(10) 0.0387(10) Uani 1 d . . .
C3 C 0.5597(4) 0.5559(10) 0.0142(5) 0.0264(15) Uani 1 d . . .
C8 C 0.1658(3) 1.1870(12) 0.3453(11) 0.0507(16) Uani 1 d D . .
C4 C 0.4837(4) 0.3368(10) 0.0152(6) 0.0259(12) Uani 1 d . . .
C1 C 0.5166(4) 0.6853(9) 0.1684(6) 0.0245(13) Uani 1 d . . .
Li1 Li 0.4321(5) 0.7267(14) 0.3404(13) 0.0347(15) Uani 1 d . . .
C5 C 0.4254(4) 0.3074(9) 0.0922(7) 0.0286(14) Uani 1 d . . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
Cl2 C5 1.737(5) . ?
Cl1 C2 1.723(5) . ?
O1 C1 1.185(8) . ?
O1 Li1 2.092(18) . ?
O2 C3 1.316(9) . ?
O2 Li1 2.097(16) 2_664 ?
O2 H 0.85(2) . ?
O3 C4 1.271(8) . ?
O3 Li1 1.997(16) 2_664 ?
O4 C6 1.253(9) . ?
O4 Li1 2.046(15) . ?
O5 C7 1.451(5) . ?
O5 Li1 2.001(8) . ?
O5 H5 0.82(2) . ?
C2 C3 1.332(11) . ?
C2 C1 1.464(11) . ?
C6 C5 1.398(11) . ?
C6 C1 1.545(7) . ?
C7 C8 1.498(7) . ?
C7 H7A 1.01(8) . ?
C7 H7B 1.00(6) . ?
C3 C4 1.508(8) . ?
C8 H8C 0.97(2) . ?
C8 H8A 0.956(19) . ?
C8 H8B 0.95(2) . ?
C4 C5 1.393(11) . ?
C1 Li1 2.79(2) . ?
Li1 O3 1.997(16) 2_665 ?
Li1 O2 2.097(16) 2_665 ?

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
C1 O1 Li1 113.8(5) . . ?
C3 O2 Li1 115.6(5) . 2_664 ?
C3 O2 H 124(4) . . ?
Li1 O2 H 115(4) 2_664 . ?
C4 O3 Li1 118.7(5) . 2_664 ?
C6 O4 Li1 115.5(5) . . ?
C7 O5 Li1 118.1(3) . . ?
C7 O5 H5 110(5) . . ?
Li1 O5 H5 112(5) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 Cl1 121.2(6) . . ?
C1 C2 Cl1 118.2(5) . . ?
O4 C6 C5 128.5(5) . . ?
O4 C6 C1 113.7(6) . . ?
C5 C6 C1 117.8(7) . . ?
O5 C7 C8 110.9(4) . . ?
O5 C7 H7A 120(5) . . ?
C8 C7 H7A 120(4) . . ?
O5 C7 H7B 94(3) . . ?
C8 C7 H7B 109(3) . . ?
H7A C7 H7B 97(6) . . ?
O2 C3 C2 125.8(5) . . ?
O2 C3 C4 112.2(6) . . ?
C2 C3 C4 122.0(7) . . ?
C7 C8 H8C 102(5) . . ?
C7 C8 H8A 114(3) . . ?
H8C C8 H8A 105(4) . . ?
C7 C8 H8B 123(5) . . ?
H8C C8 H8B 102(4) . . ?
H8A C8 H8B 108(4) . . ?
O3 C4 C5 125.2(5) . . ?
O3 C4 C3 116.0(6) . . ?
C5 C4 C3 118.8(6) . . ?
O1 C1 C2 123.4(5) . . ?
O1 C1 C6 118.5(6) . . ?
C2 C1 C6 118.1(6) . . ?
O1 C1 Li1 43.3(3) . . ?
C2 C1 Li1 166.7(4) . . ?
C6 C1 Li1 75.2(4) . . ?
O3 Li1 O5 105.7(7) 2_665 . ?
O3 Li1 O4 145.3(4) 2_665 . ?
O5 Li1 O4 108.4(6) . . ?
O3 Li1 O1 98.2(3) 2_665 . ?
O5 Li1 O1 105.6(6) . . ?
O4 Li1 O1 78.5(7) . . ?
O3 Li1 O2 77.5(7) 2_665 2_665 ?
O5 Li1 O2 108.5(7) . 2_665 ?
O4 Li1 O2 86.2(3) . 2_665 ?
O1 Li1 O2 145.6(5) . 2_665 ?
O3 Li1 C1 116.4(5) 2_665 . ?
O5 Li1 C1 110.7(7) . . ?
O4 Li1 C1 55.6(5) . . ?
O1 Li1 C1 22.9(3) . . ?
O2 Li1 C1 131.8(5) 2_665 . ?
C4 C5 C6 122.7(5) . . ?
C4 C5 Cl2 118.4(6) . . ?
C6 C5 Cl2 118.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Li1 O4 C6 C5 -179.2(6) . . . . ?
Li1 O4 C6 C1 1.5(7) . . . . ?
Li1 O5 C7 C8 177.9(11) . . . . ?
Li1 O2 C3 C2 177.1(6) 2_664 . . . ?
Li1 O2 C3 C4 -1.7(7) 2_664 . . . ?
C1 C2 C3 O2 179.4(6) . . . . ?
Cl1 C2 C3 O2 -0.9(9) . . . . ?
C1 C2 C3 C4 -1.9(8) . . . . ?
Cl1 C2 C3 C4 177.8(4) . . . . ?
Li1 O3 C4 C5 179.5(6) 2_664 . . . ?
Li1 O3 C4 C3 0.8(8) 2_664 . . . ?
O2 C3 C4 O3 0.7(8) . . . . ?
C2 C3 C4 O3 -178.2(6) . . . . ?
O2 C3 C4 C5 -178.1(6) . . . . ?
C2 C3 C4 C5 3.0(8) . . . . ?
Li1 O1 C1 C2 -179.2(5) . . . . ?
Li1 O1 C1 C6 1.4(7) . . . . ?
C3 C2 C1 O1 -178.5(6) . . . . ?
Cl1 C2 C1 O1 1.7(9) . . . . ?
C3 C2 C1 C6 0.9(8) . . . . ?
Cl1 C2 C1 C6 -178.9(4) . . . . ?
C3 C2 C1 Li1 179.2(17) . . . . ?
Cl1 C2 C1 Li1 -1(2) . . . . ?
O4 C6 C1 O1 -2.0(8) . . . . ?
C5 C6 C1 O1 178.6(6) . . . . ?
O4 C6 C1 C2 178.6(5) . . . . ?
C5 C6 C1 C2 -0.8(7) . . . . ?
O4 C6 C1 Li1 -1.0(5) . . . . ?
C5 C6 C1 Li1 179.6(5) . . . . ?
C7 O5 Li1 O3 -130.1(8) . . . 2_665 ?
C7 O5 Li1 O4 43.8(11) . . . . ?
C7 O5 Li1 O1 126.6(8) . . . . ?
C7 O5 Li1 O2 -48.3(11) . . . 2_665 ?
C7 O5 Li1 C1 103.1(8) . . . . ?
C6 O4 Li1 O3 -88.4(15) . . . 2_665 ?
C6 O4 Li1 O5 102.0(7) . . . . ?
C6 O4 Li1 O1 -0.7(5) . . . . ?
C6 O4 Li1 O2 -149.8(5) . . . 2_665 ?
C6 O4 Li1 C1 -0.9(4) . . . . ?
C1 O1 Li1 O3 144.5(5) . . . 2_665 ?
C1 O1 Li1 O5 -106.6(6) . . . . ?
C1 O1 Li1 O4 -0.4(6) . . . . ?
C1 O1 Li1 O2 64.8(14) . . . 2_665 ?
O1 C1 Li1 O3 -39.9(6) . . . 2_665 ?
C2 C1 Li1 O3 -37(2) . . . 2_665 ?
C6 C1 Li1 O3 141.3(5) . . . 2_665 ?
O1 C1 Li1 O5 80.8(5) . . . . ?
C2 C1 Li1 O5 84(2) . . . . ?
C6 C1 Li1 O5 -97.9(5) . . . . ?
O1 C1 Li1 O4 179.5(7) . . . . ?
C2 C1 Li1 O4 -178(2) . . . . ?
C6 C1 Li1 O4 0.7(3) . . . . ?
C2 C1 Li1 O1 2.8(19) . . . . ?
C6 C1 Li1 O1 -178.8(7) . . . . ?
O1 C1 Li1 O2 -136.7(8) . . . 2_665 ?
C2 C1 Li1 O2 -133.9(18) . . . 2_665 ?
C6 C1 Li1 O2 44.5(6) . . . 2_665 ?
O3 C4 C5 C6 178.3(6) . . . . ?
C3 C4 C5 C6 -3.0(8) . . . . ?
O3 C4 C5 Cl2 0.3(9) . . . . ?
C3 C4 C5 Cl2 179.0(4) . . . . ?
O4 C6 C5 C4 -177.3(6) . . . . ?
C1 C6 C5 C4 2.0(8) . . . . ?
O4 C6 C5 Cl2 0.7(9) . . . . ?
C1 C6 C5 Cl2 180.0(4) . . . . ?

data_NH4HCAx2H2O
_database_code_depnum_ccdc_archive 'CCDC 669454'

_audit_creation_date             2007-11-07T14:30:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C6 H9 Cl2 N O6'
_chemical_formula_sum            'C6 H9 Cl2 N O6'
_chemical_formula_weight         262.04
_chemical_absolute_configuration unk

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   9.5958(6)
_cell_length_b                   16.1908(14)
_cell_length_c                   6.6678(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.000(9)
_cell_angle_gamma                90
_cell_volume                     1025.85(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      5.4
_cell_measurement_theta_max      20.9

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    5.857
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.6372
_exptl_absorpt_correction_T_max  0.7394

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        5
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 -6 0
-4 -2 1
-1 1 2

_diffrn_reflns_number            1165
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         5.4
_diffrn_reflns_theta_max         76.21
_diffrn_reflns_theta_full        76.21
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_reflns_number_total             1165
_reflns_number_gt                965
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.0550P)²+0.2697P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_number_reflns         1165
_refine_ls_number_parameters     169
_refine_ls_number_restraints     19
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0893
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(7)
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.337

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Cl2 Cl 0.32740(15) 0.34038(12) 0.2356(2) 0.0431(7) Uani 1 d . . .
Cl1 Cl 0.71056(14) 0.65991(13) 0.3438(2) 0.0434(7) Uani 1 d . . .
O1 O 0.4006(8) 0.6511(4) 0.2521(14) 0.0399(18) Uani 1 d . . .
O3 O 0.6401(8) 0.3507(4) 0.3273(14) 0.0391(18) Uani 1 d . . .
O2 O 0.8015(7) 0.4798(5) 0.3813(14) 0.0425(19) Uani 1 d D . .
O4 O 0.2376(7) 0.5191(5) 0.2009(15) 0.045(2) Uani 1 d . . .
C4 C 0.5749(10) 0.4183(6) 0.3088(15) 0.035(2) Uani 1 d . . .
O6 O 0.9347(7) 0.6804(5) 0.8458(12) 0.044(2) Uani 1 d D . .
N1 N 1.1006(9) 0.6784(6) 0.2295(16) 0.044(2) Uani 1 d D . .
C6 C 0.3663(9) 0.5076(5) 0.2412(17) 0.030(2) Uani 1 d . . .
C1 C 0.4579(7) 0.5824(5) 0.2711(14) 0.0257(18) Uani 1 d . . .
C3 C 0.6687(9) 0.4977(5) 0.3365(17) 0.030(2) Uani 1 d . . .
O5 O 1.0196(10) 0.57803(17) 0.531(2) 0.0481(9) Uani 1 d D . .
C5 C 0.4319(10) 0.4274(4) 0.2674(16) 0.032(2) Uani 1 d . . .
C2 C 0.6084(9) 0.5719(5) 0.3168(15) 0.032(2) Uani 1 d . . .
H1B H 1.028(4) 0.676(3) 0.122(5) 0.06 Uiso 1 d D . .
H6B H 0.840(3) 0.670(4) 0.842(12) 0.06 Uiso 1 d D . .
H6A H 0.946(7) 0.736(2) 0.813(13) 0.08(2) Uiso 1 d D . .
H5A H 1.099(4) 0.547(3) 0.592(8) 0.06 Uiso 1 d D . .
H1A H 1.109(6) 0.7312(18) 0.276(9) 0.06 Uiso 1 d D . .
H1 H 0.870(5) 0.511(4) 0.404(15) 0.13(3) Uiso 1 d D . .
H1C H 1.071(5) 0.645(3) 0.327(6) 0.060(17) Uiso 1 d D . .
H1D H 1.178(4) 0.656(4) 0.187(9) 0.09(3) Uiso 1 d D . .
H5B H 0.994(8) 0.607(4) 0.645(8) 0.12(3) Uiso 1 d D . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
Cl2 C5 1.725(8) . ?
Cl1 C2 1.725(9) . ?
O1 C1 1.239(11) . ?
O3 C4 1.258(11) . ?
O2 C3 1.301(11) . ?
O2 H1 0.83(2) . ?
O4 C6 1.241(11) . ?
C4 C5 1.369(12) . ?
C4 C3 1.566(12) . ?
O6 H6B 0.93(2) . ?
O6 H6A 0.94(2) . ?
N1 H1B 0.929(19) . ?
N1 H1A 0.910(18) . ?
N1 H1C 0.924(19) . ?
N1 H1D 0.909(19) . ?
C6 C5 1.444(11) . ?
C6 C1 1.494(12) . ?
C1 C2 1.444(10) . ?
C3 C2 1.331(12) . ?
O5 H5A 0.96(2) . ?
O5 H5B 0.96(2) . ?

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 O2 H1 130(6) . . ?
O3 C4 C5 125.7(9) . . ?
O3 C4 C3 115.7(7) . . ?
C5 C4 C3 118.6(8) . . ?
H6B O6 H6A 108(4) . . ?
H1B N1 H1A 109(4) . . ?
H1B N1 H1C 104(3) . . ?
H1A N1 H1C 109(4) . . ?
H1B N1 H1D 107(4) . . ?
H1A N1 H1D 117(4) . . ?
H1C N1 H1D 109(4) . . ?
O4 C6 C5 124.4(8) . . ?
O4 C6 C1 117.2(7) . . ?
C5 C6 C1 118.4(7) . . ?
O1 C1 C2 123.0(7) . . ?
O1 C1 C6 118.0(6) . . ?
C2 C1 C6 119.0(7) . . ?
O2 C3 C2 128.5(7) . . ?
O2 C3 C4 111.8(7) . . ?
C2 C3 C4 119.6(7) . . ?
H5A O5 H5B 102(4) . . ?
C4 C5 C6 122.0(7) . . ?
C4 C5 Cl2 119.1(7) . . ?
C6 C5 Cl2 118.9(7) . . ?
C3 C2 C1 122.4(8) . . ?
C3 C2 Cl1 120.1(6) . . ?
C1 C2 Cl1 117.5(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 C6 C1 O1 -0.7(14) . . . . ?
C5 C6 C1 O1 -178.7(10) . . . . ?
O4 C6 C1 C2 -179.6(10) . . . . ?
C5 C6 C1 C2 2.5(12) . . . . ?
O3 C4 C3 O2 -2.0(12) . . . . ?
C5 C4 C3 O2 178.0(10) . . . . ?
O3 C4 C3 C2 179.1(11) . . . . ?
C5 C4 C3 C2 -0.9(12) . . . . ?
O3 C4 C5 C6 -177.6(9) . . . . ?
C3 C4 C5 C6 2.4(13) . . . . ?
O3 C4 C5 Cl2 -0.3(15) . . . . ?
C3 C4 C5 Cl2 179.8(7) . . . . ?
O4 C6 C5 C4 179.0(10) . . . . ?
C1 C6 C5 C4 -3.2(14) . . . . ?
O4 C6 C5 Cl2 1.6(16) . . . . ?
C1 C6 C5 Cl2 179.4(7) . . . . ?
O2 C3 C2 C1 -178.4(10) . . . . ?
C4 C3 C2 C1 0.3(14) . . . . ?
O2 C3 C2 Cl1 2.1(17) . . . . ?
C4 C3 C2 Cl1 -179.2(7) . . . . ?
O1 C1 C2 C3 -179.9(9) . . . . ?
C6 C1 C2 C3 -1.1(13) . . . . ?
O1 C1 C2 Cl1 -0.4(14) . . . . ?
C6 C1 C2 Cl1 178.4(7) . . . . ?
#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_Na5HCA(CA)2(H2O)10
_database_code_depnum_ccdc_archive 'CCDC 669455'

_audit_creation_date             2007-10-04T11:22:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C18 H21 Cl6 Na5 O22'
_chemical_formula_sum            'C18 H21 Cl6 Na5 O22'
_chemical_formula_weight         917.01

#------------------ UNIT CELL INFORMATION -----------------------------------#

_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                   10.87270(10)
_cell_length_b                   12.99730(10)
_cell_length_c                   13.3899(2)
_cell_angle_alpha                67.0940(10)
_cell_angle_beta                 66.5280(10)
_cell_angle_gamma                74.3590(10)
_cell_volume                     1584.00(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10433
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      33.14

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             924
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_type   none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_ambient_temperature      150.0(10)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       
;
ω scans at κ=55°
;
_diffrn_detector_area_resol_mean 0.055
_diffrn_radiation_probe          x-ray
_diffrn_reflns_number            20083
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         33.12
_diffrn_reflns_theta_full        33.12
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_reflns_number_total             11811
_reflns_number_gt                9399
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.0290P)²+0.4289P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0017(6)
_refine_ls_number_reflns         11811
_refine_ls_number_parameters     543
_refine_ls_number_restraints     31
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0796
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.013
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.513

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
O21 O 0.99677(11) 0.68518(10) 0.57018(10) 0.0319(2) Uani 1 d D . .
C4 C 0.43611(11) 0.47133(9) 0.69789(9) 0.01127(18) Uani 1 d . . .
Cl6 Cl 0.61454(3) 1.42582(2) 0.06934(2) 0.01488(6) Uani 1 d . . .
Cl5 Cl 0.89264(3) 1.07432(2) 0.43000(2) 0.01766(6) Uani 1 d . . .
O12 O 0.89085(8) 1.41592(7) 0.07652(7) 0.01562(15) Uani 1 d . . .
O11 O 1.00497(8) 1.26933(7) 0.22999(8) 0.01883(17) Uani 1 d . . .
O9 O 0.50457(8) 1.23027(7) 0.26893(7) 0.01845(17) Uani 1 d . . .
C13 C 0.62067(10) 1.24397(9) 0.25532(9) 0.01105(18) Uani 1 d . . .
O10 O 0.61858(8) 1.08361(7) 0.42039(7) 0.01580(16) Uani 1 d . . .
C15 C 0.81793(10) 1.16916(9) 0.33036(9) 0.01147(18) Uani 1 d . . .
C16 C 0.88955(10) 1.25554(9) 0.24225(9) 0.01150(18) Uani 1 d . . .
C17 C 0.82318(10) 1.34147(8) 0.15384(9) 0.01059(18) Uani 1 d . . .
C18 C 0.69167(10) 1.33027(9) 0.16780(9) 0.01102(18) Uani 1 d . . .
C14 C 0.68750(10) 1.15836(9) 0.34282(9) 0.01081(18) Uani 1 d . . .
Cl3 Cl 1.15695(3) 0.87402(2) 0.27619(2) 0.01683(6) Uani 1 d . . .
Cl2 Cl 0.63218(3) 0.37652(2) 0.79215(2) 0.01585(6) Uani 1 d . . .
Cl1 Cl 0.37546(3) 0.73788(2) 0.42278(2) 0.01504(6) Uani 1 d . . .
Cl4 Cl 0.85888(3) 1.23685(2) -0.06363(2) 0.01320(5) Uani 1 d . . .
Na2 Na 0.69047(4) 0.85381(4) 0.24638(4) 0.01499(9) Uani 1 d . . .
O24 O 0.50133(8) 0.96929(7) 0.33310(7) 0.01536(15) Uani 1 d D . .
O25 O 0.53843(8) 1.13569(7) 0.05882(8) 0.01736(16) Uani 1 d D . .
O29 O -0.07612(8) 1.56954(7) 0.21464(7) 0.01609(16) Uani 1 d D . .
O8 O 1.14704(8) 1.21695(7) -0.07489(7) 0.01517(15) Uani 1 d . . .
O3 O 0.36444(8) 0.39821(7) 0.77183(7) 0.01559(15) Uani 1 d . . .
O5 O 0.75855(8) 1.03389(7) 0.12915(7) 0.01561(16) Uani 1 d . . .
O6 O 0.88335(8) 0.87991(7) 0.27156(7) 0.01492(15) Uani 1 d . . .
O4 O 0.76892(8) 0.56118(7) 0.58127(7) 0.01734(16) Uani 1 d . . .
O1 O 0.65943(8) 0.70588(7) 0.42286(7) 0.01574(16) Uani 1 d . . .
O2 O 0.24980(8) 0.55576(7) 0.62488(7) 0.01612(16) Uani 1 d D . .
O7 O 1.26845(8) 1.06655(7) 0.07056(7) 0.01521(15) Uani 1 d . . .
C10 C 1.14844(10) 1.05658(9) 0.09015(9) 0.01055(18) Uani 1 d . . .
C8 C 0.94615(10) 0.95883(9) 0.19696(9) 0.01081(18) Uani 1 d . . .
C3 C 0.37485(10) 0.56048(9) 0.61114(9) 0.01110(18) Uani 1 d . . .
C5 C 0.56809(10) 0.47697(9) 0.68783(9) 0.01192(18) Uani 1 d . . .
C9 C 1.07660(10) 0.97293(9) 0.18184(9) 0.01114(18) Uani 1 d . . .
C6 C 0.64912(10) 0.55469(9) 0.59711(9) 0.01187(18) Uani 1 d . . .
C11 C 1.07745(10) 1.14429(8) 0.00650(9) 0.01034(18) Uani 1 d . . .
C12 C 0.94332(10) 1.13681(8) 0.02637(9) 0.01040(18) Uani 1 d . . .
C7 C 0.87469(10) 1.04797(9) 0.11362(9) 0.01037(18) Uani 1 d . . .
C2 C 0.44745(10) 0.63960(9) 0.52167(9) 0.01131(18) Uani 1 d . . .
C1 C 0.58673(10) 0.64067(8) 0.50587(9) 0.01119(18) Uani 1 d . . .
Na5 Na 0.08334(4) 1.44651(4) 0.10119(4) 0.01423(9) Uani 1 d . . .
Na1 Na 0.86727(5) 0.73087(4) 0.44807(4) 0.01509(9) Uani 1 d . . .
Na3 Na 0.38944(5) 1.00043(4) 0.19937(4) 0.01517(9) Uani 1 d . . .
Na4 Na 0.39061(5) 1.27718(4) 0.13876(4) 0.01720(10) Uani 1 d . . .
O27 O 0.26939(8) 1.32573(7) 0.01293(7) 0.01562(15) Uani 1 d D . .
O22 O 0.70901(8) 0.85642(7) 0.53667(7) 0.01602(16) Uani 1 d D . .
O26 O 0.24364(8) 1.14039(7) 0.27448(8) 0.01781(16) Uani 1 d D . .
O20 O 1.03926(9) 0.61713(8) 0.34539(8) 0.01979(17) Uani 1 d D . .
O23 O 0.54614(8) 0.85090(7) 0.14110(7) 0.01593(16) Uani 1 d D . .
O28 O 0.22391(11) 1.41711(10) 0.21056(10) 0.0317(2) Uani 1 d D . .
H23B H 0.6152(15) 0.8696(13) 0.0731(12) 0.030(4) Uiso 1 d D . .
H23A H 0.5518(17) 0.7776(11) 0.1661(14) 0.032(5) Uiso 1 d D . .
H27B H 0.3055(18) 1.3657(14) -0.0606(12) 0.041(5) Uiso 1 d D . .
H22B H 0.6918(16) 0.9278(11) 0.4922(13) 0.031(4) Uiso 1 d D . .
H22A H 0.6283(15) 0.8368(14) 0.5862(14) 0.039(5) Uiso 1 d D . .
H29B H -0.0389(17) 1.5836(14) 0.2563(14) 0.04 Uiso 1 d D . .
H26B H 0.1593(15) 1.1659(15) 0.2734(16) 0.043(5) Uiso 1 d D . .
H26A H 0.242(2) 1.1349(17) 0.3460(14) 0.053(6) Uiso 1 d D . .
H20A H 1.0946(18) 0.5550(13) 0.3701(16) 0.049(6) Uiso 1 d D . .
H29A H -0.0976(16) 1.6361(11) 0.1671(13) 0.033(5) Uiso 1 d D . .
H25B H 0.5494(19) 1.1434(16) -0.0126(13) 0.049(6) Uiso 1 d D . .
H24B H 0.5302(18) 1.0281(13) 0.3291(16) 0.045(5) Uiso 1 d D . .
H25A H 0.6226(16) 1.1118(16) 0.0629(17) 0.054(6) Uiso 1 d D . .
H H 0.208(2) 0.5043(16) 0.6872(16) 0.071(7) Uiso 1 d D . .
H24A H 0.4612(19) 0.9377(15) 0.4071(13) 0.050(6) Uiso 1 d D . .
H27A H 0.242(2) 1.2691(14) 0.0095(17) 0.055(6) Uiso 1 d D . .
H20B H 1.0923(19) 0.6707(14) 0.2900(15) 0.055(6) Uiso 1 d D . .
H21A H 1.073(2) 0.6363(19) 0.564(2) 0.095(9) Uiso 1 d D . .
H28A H 0.169(2) 1.3894(18) 0.2828(14) 0.068(7) Uiso 1 d D . .
H21B H 1.004(3) 0.7313(19) 0.601(2) 0.098(9) Uiso 1 d D . .
H28B H 0.2516(19) 1.4759(14) 0.2122(17) 0.05 Uiso 1 d D . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
O21 Na1 2.3740(11) . ?
O21 H21A 0.891(16) . ?
O21 H21B 0.886(16) . ?
C4 O3 1.2422(13) . ?
C4 C5 1.4063(14) . ?
C4 C3 1.5126(14) . ?
Cl6 C18 1.7401(10) . ?
Cl6 Na4 3.1400(5) . ?
Cl5 C15 1.7328(10) . ?
O12 C17 1.2437(12) . ?
O12 Na5 2.3162(9) 2_685 ?
O12 Na5 2.3976(9) 1_655 ?
O11 C16 1.2522(12) . ?
O11 Na5 2.4082(9) 1_655 ?
O9 C13 1.2534(12) . ?
O9 Na4 2.3304(9) . ?
C13 C18 1.3965(14) . ?
C13 C14 1.5383(14) . ?
O10 C14 1.2535(12) . ?
C15 C14 1.3997(14) . ?
C15 C16 1.4026(14) . ?
C16 C17 1.5448(14) . ?
C17 C18 1.4067(14) . ?
Cl3 C9 1.7382(10) . ?
Cl3 Na3 3.0000(5) 1_655 ?
Cl2 C5 1.7338(10) . ?
Cl1 C2 1.7227(10) . ?
Cl4 C12 1.7332(10) . ?
Na2 O1 2.3607(9) . ?
Na2 O24 2.3708(9) . ?
Na2 O5 2.3746(9) . ?
Na2 O6 2.3796(9) . ?
Na2 O23 2.5073(9) . ?
Na2 O8 2.6030(10) 2_775 ?
Na2 Na3 3.4763(6) . ?
Na2 Na1 3.5583(6) . ?
Na2 H23B 2.673(16) . ?
O24 Na3 2.3992(9) . ?
O24 H24B 0.878(14) . ?
O24 H24A 0.881(14) . ?
O25 Na4 2.3831(10) . ?
O25 Na3 2.4058(10) . ?
O25 H25B 0.883(14) . ?
O25 H25A 0.900(14) . ?
O29 Na5 2.4836(10) . ?
O29 H29B 0.899(14) . ?
O29 H29A 0.888(13) . ?
O8 C11 1.2567(12) . ?
O8 Na2 2.6030(10) 2_775 ?
O5 C7 1.2478(12) . ?
O6 C8 1.2461(12) . ?
O6 Na1 2.3788(9) . ?
O4 C6 1.2546(12) . ?
O4 Na1 2.4246(9) . ?
O1 C1 1.2274(13) . ?
O1 Na1 2.5327(9) . ?
O2 C3 1.3127(12) . ?
O2 H 0.882(15) . ?
O7 C10 1.2570(12) . ?
O7 Na3 2.3426(9) 1_655 ?
C10 C9 1.3980(14) . ?
C10 C11 1.5395(14) . ?
C8 C9 1.4032(14) . ?
C8 C7 1.5460(14) . ?
C3 C2 1.3569(14) . ?
C5 C6 1.3945(14) . ?
C6 C1 1.5460(15) . ?
C11 C12 1.3980(14) . ?
C12 C7 1.4054(14) . ?
C2 C1 1.4463(14) . ?
Na5 O12 2.3162(9) 2_685 ?
Na5 O28 2.3789(11) . ?
Na5 O12 2.3976(9) 1_455 ?
Na5 O27 2.4043(9) . ?
Na5 O11 2.4082(9) 1_455 ?
Na5 Na5 3.4901(9) 2_585 ?
Na5 Na4 3.5736(6) . ?
Na1 O22 2.3234(9) . ?
Na1 O20 2.3698(10) . ?
Na3 O26 2.3309(9) . ?
Na3 O7 2.3426(9) 1_455 ?
Na3 O23 2.3716(9) . ?
Na3 Cl3 3.0000(5) 1_455 ?
Na3 Na4 3.3676(7) . ?
Na4 O27 2.3382(9) . ?
Na4 O28 2.3901(11) . ?
Na4 O26 2.3917(10) . ?
O27 H27B 0.893(14) . ?
O27 H27A 0.888(14) . ?
O22 H22B 0.903(13) . ?
O22 H22A 0.894(13) . ?
O26 H26B 0.891(14) . ?
O26 H26A 0.925(14) . ?
O20 H20A 0.901(14) . ?
O20 H20B 0.917(14) . ?
O23 H23B 0.913(13) . ?
O23 H23A 0.872(13) . ?
O28 H28A 0.898(15) . ?
O28 H28B 0.904(14) . ?

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
Na1 O21 H21A 122.5(17) . . ?
Na1 O21 H21B 125.4(17) . . ?
H21A O21 H21B 106(2) . . ?
O3 C4 C5 125.67(10) . . ?
O3 C4 C3 116.24(9) . . ?
C5 C4 C3 118.08(9) . . ?
C18 Cl6 Na4 94.70(4) . . ?
C17 O12 Na5 146.36(7) . 2_685 ?
C17 O12 Na5 118.13(7) . 1_655 ?
Na5 O12 Na5 95.52(3) 2_685 1_655 ?
C16 O11 Na5 117.66(7) . 1_655 ?
C13 O9 Na4 131.63(7) . . ?
O9 C13 C18 124.86(10) . . ?
O9 C13 C14 116.43(9) . . ?
C18 C13 C14 118.71(9) . . ?
C14 C15 C16 122.75(9) . . ?
C14 C15 Cl5 118.80(8) . . ?
C16 C15 Cl5 118.43(8) . . ?
O11 C16 C15 124.50(10) . . ?
O11 C16 C17 116.62(9) . . ?
C15 C16 C17 118.88(9) . . ?
O12 C17 C18 125.46(10) . . ?
O12 C17 C16 116.70(9) . . ?
C18 C17 C16 117.83(9) . . ?
C13 C18 C17 123.21(9) . . ?
C13 C18 Cl6 117.96(8) . . ?
C17 C18 Cl6 118.81(8) . . ?
O10 C14 C15 125.38(10) . . ?
O10 C14 C13 116.02(9) . . ?
C15 C14 C13 118.60(9) . . ?
C9 Cl3 Na3 95.99(4) . 1_655 ?
O1 Na2 O24 91.01(3) . . ?
O1 Na2 O5 149.32(4) . . ?
O24 Na2 O5 80.40(3) . . ?
O1 Na2 O6 86.87(3) . . ?
O24 Na2 O6 107.61(3) . . ?
O5 Na2 O6 68.22(3) . . ?
O1 Na2 O23 111.60(3) . . ?
O24 Na2 O23 85.10(3) . . ?
O5 Na2 O23 97.05(3) . . ?
O6 Na2 O23 157.78(3) . . ?
O1 Na2 O8 111.40(3) . 2_775 ?
O24 Na2 O8 153.32(3) . 2_775 ?
O5 Na2 O8 86.48(3) . 2_775 ?
O6 Na2 O8 88.56(3) . 2_775 ?
O23 Na2 O8 73.52(3) . 2_775 ?
O1 Na2 Na3 113.68(3) . . ?
O24 Na2 Na3 43.54(2) . . ?
O5 Na2 Na3 79.78(2) . . ?
O6 Na2 Na3 141.23(3) . . ?
O23 Na2 Na3 43.01(2) . . ?
O8 Na2 Na3 111.37(2) 2_775 . ?
O1 Na2 Na1 45.29(2) . . ?
O24 Na2 Na1 103.85(3) . . ?
O5 Na2 Na1 108.14(2) . . ?
O6 Na2 Na1 41.59(2) . . ?
O23 Na2 Na1 154.27(3) . . ?
O8 Na2 Na1 102.28(2) 2_775 . ?
Na3 Na2 Na1 145.932(18) . . ?
O1 Na2 H23B 126.2(3) . . ?
O24 Na2 H23B 98.1(3) . . ?
O5 Na2 H23B 84.3(3) . . ?
O6 Na2 H23B 137.8(3) . . ?
O23 Na2 H23B 20.0(3) . . ?
O8 Na2 H23B 57.3(3) 2_775 . ?
Na3 Na2 H23B 54.6(3) . . ?
Na1 Na2 H23B 156.2(3) . . ?
Na2 O24 Na3 93.57(3) . . ?
Na2 O24 H24B 108.1(12) . . ?
Na3 O24 H24B 116.3(12) . . ?
Na2 O24 H24A 114.4(13) . . ?
Na3 O24 H24A 119.8(13) . . ?
H24B O24 H24A 104.4(16) . . ?
Na4 O25 Na3 89.37(3) . . ?
Na4 O25 H25B 118.2(13) . . ?
Na3 O25 H25B 113.1(12) . . ?
Na4 O25 H25A 121.8(13) . . ?
Na3 O25 H25A 110.2(13) . . ?
H25B O25 H25A 103.7(16) . . ?
Na5 O29 H29B 112.2(11) . . ?
Na5 O29 H29A 109.3(10) . . ?
H29B O29 H29A 106.0(14) . . ?
C11 O8 Na2 113.80(7) . 2_775 ?
C7 O5 Na2 117.55(7) . . ?
C8 O6 Na1 146.19(7) . . ?
C8 O6 Na2 116.99(7) . . ?
Na1 O6 Na2 96.80(3) . . ?
C6 O4 Na1 119.54(7) . . ?
C1 O1 Na2 149.83(7) . . ?
C1 O1 Na1 115.71(7) . . ?
Na2 O1 Na1 93.23(3) . . ?
C3 O2 H 116.2(15) . . ?
C10 O7 Na3 128.42(7) . 1_655 ?
O7 C10 C9 124.65(10) . . ?
O7 C10 C11 116.58(9) . . ?
C9 C10 C11 118.77(9) . . ?
O6 C8 C9 125.42(10) . . ?
O6 C8 C7 117.19(9) . . ?
C9 C8 C7 117.39(9) . . ?
O2 C3 C2 121.78(9) . . ?
O2 C3 C4 116.89(9) . . ?
C2 C3 C4 121.31(9) . . ?
C6 C5 C4 123.45(9) . . ?
C6 C5 Cl2 119.83(8) . . ?
C4 C5 Cl2 116.66(8) . . ?
C10 C9 C8 123.41(9) . . ?
C10 C9 Cl3 118.69(8) . . ?
C8 C9 Cl3 117.71(8) . . ?
O4 C6 C5 126.36(10) . . ?
O4 C6 C1 116.39(9) . . ?
C5 C6 C1 117.24(9) . . ?
O8 C11 C12 125.66(10) . . ?
O8 C11 C10 116.11(9) . . ?
C12 C11 C10 118.23(9) . . ?
C11 C12 C7 122.77(9) . . ?
C11 C12 Cl4 119.35(8) . . ?
C7 C12 Cl4 117.81(7) . . ?
O5 C7 C12 124.78(9) . . ?
O5 C7 C8 116.18(9) . . ?
C12 C7 C8 119.03(8) . . ?
C3 C2 C1 120.83(9) . . ?
C3 C2 Cl1 119.99(8) . . ?
C1 C2 Cl1 119.16(8) . . ?
O1 C1 C2 123.51(10) . . ?
O1 C1 C6 117.67(9) . . ?
C2 C1 C6 118.82(9) . . ?
O12 Na5 O28 122.28(4) 2_685 . ?
O12 Na5 O12 84.48(3) 2_685 1_455 ?
O28 Na5 O12 152.91(4) . 1_455 ?
O12 Na5 O27 89.88(3) 2_685 . ?
O28 Na5 O27 81.48(3) . . ?
O12 Na5 O27 104.53(3) 1_455 . ?
O12 Na5 O11 147.65(4) 2_685 1_455 ?
O28 Na5 O11 87.74(4) . 1_455 ?
O12 Na5 O11 67.35(3) 1_455 1_455 ?
O27 Na5 O11 82.52(3) . 1_455 ?
O12 Na5 O29 95.67(3) 2_685 . ?
O28 Na5 O29 86.12(3) . . ?
O12 Na5 O29 87.15(3) 1_455 . ?
O27 Na5 O29 167.53(3) . . ?
O11 Na5 O29 98.37(3) 1_455 . ?
O12 Na5 Na5 43.14(2) 2_685 2_585 ?
O28 Na5 Na5 165.03(4) . 2_585 ?
O12 Na5 Na5 41.34(2) 1_455 2_585 ?
O27 Na5 Na5 99.85(3) . 2_585 ?
O11 Na5 Na5 107.22(3) 1_455 2_585 ?
O29 Na5 Na5 91.80(3) . 2_585 ?
O12 Na5 Na4 114.80(3) 2_685 . ?
O28 Na5 Na4 41.59(3) . . ?
O12 Na5 Na4 134.95(3) 1_455 . ?
O27 Na5 Na4 40.41(2) . . ?
O11 Na5 Na4 78.49(2) 1_455 . ?
O29 Na5 Na4 127.41(3) . . ?
Na5 Na5 Na4 139.79(2) 2_585 . ?
O22 Na1 O20 174.72(4) . . ?
O22 Na1 O21 92.58(4) . . ?
O20 Na1 O21 87.70(4) . . ?
O22 Na1 O6 86.57(3) . . ?
O20 Na1 O6 89.12(3) . . ?
O21 Na1 O6 128.22(4) . . ?
O22 Na1 O4 97.17(3) . . ?
O20 Na1 O4 88.10(3) . . ?
O21 Na1 O4 84.59(4) . . ?
O6 Na1 O4 146.92(3) . . ?
O22 Na1 O1 81.07(3) . . ?
O20 Na1 O1 101.44(3) . . ?
O21 Na1 O1 147.87(4) . . ?
O6 Na1 O1 83.08(3) . . ?
O4 Na1 O1 65.25(3) . . ?
O22 Na1 Na2 82.43(3) . . ?
O20 Na1 Na2 96.35(3) . . ?
O21 Na1 Na2 168.65(4) . . ?
O6 Na1 Na2 41.61(2) . . ?
O4 Na1 Na2 106.09(2) . . ?
O1 Na1 Na2 41.48(2) . . ?
O26 Na3 O7 83.91(3) . 1_455 ?
O26 Na3 O23 173.54(4) . . ?
O7 Na3 O23 102.47(3) 1_455 . ?
O26 Na3 O24 86.19(3) . . ?
O7 Na3 O24 168.87(4) 1_455 . ?
O23 Na3 O24 87.54(3) . . ?
O26 Na3 O25 90.27(3) . . ?
O7 Na3 O25 85.51(3) 1_455 . ?
O23 Na3 O25 91.21(3) . . ?
O24 Na3 O25 89.46(3) . . ?
O26 Na3 Cl3 90.50(3) . 1_455 ?
O7 Na3 Cl3 66.69(2) 1_455 1_455 ?
O23 Na3 Cl3 91.14(2) . 1_455 ?
O24 Na3 Cl3 118.58(3) . 1_455 ?
O25 Na3 Cl3 151.94(3) . 1_455 ?
O26 Na3 Na4 45.24(2) . . ?
O7 Na3 Na4 83.22(3) 1_455 . ?
O23 Na3 Na4 135.78(3) . . ?
O24 Na3 Na4 86.20(2) . . ?
O25 Na3 Na4 45.04(2) . . ?
Cl3 Na3 Na4 129.693(18) 1_455 . ?
O26 Na3 Na2 128.01(3) . . ?
O7 Na3 Na2 145.15(3) 1_455 . ?
O23 Na3 Na2 46.15(2) . . ?
O24 Na3 Na2 42.90(2) . . ?
O25 Na3 Na2 81.30(2) . . ?
Cl3 Na3 Na2 119.303(17) 1_455 . ?
Na4 Na3 Na2 108.570(17) . . ?
O9 Na4 O27 178.04(4) . . ?
O9 Na4 O25 90.39(3) . . ?
O27 Na4 O25 91.25(3) . . ?
O9 Na4 O28 95.68(4) . . ?
O27 Na4 O28 82.63(3) . . ?
O25 Na4 O28 173.37(4) . . ?
O9 Na4 O26 89.07(3) . . ?
O27 Na4 O26 89.87(3) . . ?
O25 Na4 O26 89.37(3) . . ?
O28 Na4 O26 88.07(4) . . ?
O9 Na4 Cl6 63.83(2) . . ?
O27 Na4 Cl6 117.03(3) . . ?
O25 Na4 Cl6 96.04(3) . . ?
O28 Na4 Cl6 89.04(3) . . ?
O26 Na4 Cl6 152.31(3) . . ?
O9 Na4 Na3 88.90(3) . . ?
O27 Na4 Na3 91.48(3) . . ?
O25 Na4 Na3 45.59(2) . . ?
O28 Na4 Na3 131.65(4) . . ?
O26 Na4 Na3 43.79(2) . . ?
Cl6 Na4 Na3 134.400(18) . . ?
O9 Na4 Na5 136.38(3) . . ?
O27 Na4 Na5 41.80(2) . . ?
O25 Na4 Na5 132.22(3) . . ?
O28 Na4 Na5 41.35(3) . . ?
O26 Na4 Na5 83.47(2) . . ?
Cl6 Na4 Na5 111.627(16) . . ?
Na3 Na4 Na5 113.132(17) . . ?
Na4 O27 Na5 97.79(3) . . ?
Na4 O27 H27B 119.3(12) . . ?
Na5 O27 H27B 107.5(12) . . ?
Na4 O27 H27A 116.1(13) . . ?
Na5 O27 H27A 112.0(13) . . ?
H27B O27 H27A 104.0(16) . . ?
Na1 O22 H22B 118.1(10) . . ?
Na1 O22 H22A 120.3(11) . . ?
H22B O22 H22A 105.6(15) . . ?
Na3 O26 Na4 90.97(3) . . ?
Na3 O26 H26B 125.7(12) . . ?
Na4 O26 H26B 110.2(12) . . ?
Na3 O26 H26A 115.4(12) . . ?
Na4 O26 H26A 105.8(12) . . ?
H26B O26 H26A 106.1(16) . . ?
Na1 O20 H20A 130.1(12) . . ?
Na1 O20 H20B 99.9(12) . . ?
H20A O20 H20B 107.8(16) . . ?
Na3 O23 Na2 90.84(3) . . ?
Na3 O23 H23B 117.5(10) . . ?
Na2 O23 H23B 90.3(10) . . ?
Na3 O23 H23A 135.3(11) . . ?
Na2 O23 H23A 93.8(11) . . ?
H23B O23 H23A 106.9(14) . . ?
Na5 O28 Na4 97.06(4) . . ?
Na5 O28 H28A 102.1(15) . . ?
Na4 O28 H28A 113.7(14) . . ?
Na5 O28 H28B 120.9(13) . . ?
Na4 O28 H28B 118.8(13) . . ?
H28A O28 H28B 103.6(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Na4 O9 C13 C18 28.08(17) . . . . ?
Na4 O9 C13 C14 -152.05(8) . . . . ?
Na5 O11 C16 C15 -165.83(8) 1_655 . . . ?
Na5 O11 C16 C17 13.50(12) 1_655 . . . ?
C14 C15 C16 O11 178.29(11) . . . . ?
Cl5 C15 C16 O11 0.08(16) . . . . ?
C14 C15 C16 C17 -1.02(16) . . . . ?
Cl5 C15 C16 C17 -179.23(7) . . . . ?
Na5 O12 C17 C18 -16.7(2) 2_685 . . . ?
Na5 O12 C17 C18 163.56(8) 1_655 . . . ?
Na5 O12 C17 C16 164.09(9) 2_685 . . . ?
Na5 O12 C17 C16 -15.63(12) 1_655 . . . ?
O11 C16 C17 O12 1.35(15) . . . . ?
C15 C16 C17 O12 -179.28(10) . . . . ?
O11 C16 C17 C18 -177.90(10) . . . . ?
C15 C16 C17 C18 1.47(15) . . . . ?
O9 C13 C18 C17 -178.58(11) . . . . ?
C14 C13 C18 C17 1.56(16) . . . . ?
O9 C13 C18 Cl6 -0.42(15) . . . . ?
C14 C13 C18 Cl6 179.71(7) . . . . ?
O12 C17 C18 C13 179.04(10) . . . . ?
C16 C17 C18 C13 -1.78(16) . . . . ?
O12 C17 C18 Cl6 0.90(15) . . . . ?
C16 C17 C18 Cl6 -179.92(7) . . . . ?
Na4 Cl6 C18 C13 -14.74(9) . . . . ?
Na4 Cl6 C18 C17 163.49(8) . . . . ?
C16 C15 C14 O10 -179.30(10) . . . . ?
Cl5 C15 C14 O10 -1.10(16) . . . . ?
C16 C15 C14 C13 0.78(16) . . . . ?
Cl5 C15 C14 C13 178.98(7) . . . . ?
O9 C13 C14 O10 -0.79(15) . . . . ?
C18 C13 C14 O10 179.09(10) . . . . ?
O9 C13 C14 C15 179.14(10) . . . . ?
C18 C13 C14 C15 -0.98(15) . . . . ?
O1 Na2 O24 Na3 -124.38(3) . . . . ?
O5 Na2 O24 Na3 85.23(3) . . . . ?
O6 Na2 O24 Na3 148.59(3) . . . . ?
O23 Na2 O24 Na3 -12.78(3) . . . . ?
O8 Na2 O24 Na3 23.62(8) 2_775 . . . ?
Na1 Na2 O24 Na3 -168.29(2) . . . . ?
O1 Na2 O5 C7 54.62(11) . . . . ?
O24 Na2 O5 C7 130.13(8) . . . . ?
O6 Na2 O5 C7 16.67(8) . . . . ?
O23 Na2 O5 C7 -146.08(8) . . . . ?
O8 Na2 O5 C7 -73.18(8) 2_775 . . . ?
Na3 Na2 O5 C7 174.35(8) . . . . ?
Na1 Na2 O5 C7 28.59(8) . . . . ?
O1 Na2 O6 C8 -177.72(8) . . . . ?
O24 Na2 O6 C8 -87.65(8) . . . . ?
O5 Na2 O6 C8 -16.03(8) . . . . ?
O23 Na2 O6 C8 35.04(14) . . . . ?
O8 Na2 O6 C8 70.75(8) 2_775 . . . ?
Na3 Na2 O6 C8 -52.67(10) . . . . ?
Na1 Na2 O6 C8 -178.83(9) . . . . ?
O1 Na2 O6 Na1 1.12(3) . . . . ?
O24 Na2 O6 Na1 91.18(4) . . . . ?
O5 Na2 O6 Na1 162.80(4) . . . . ?
O23 Na2 O6 Na1 -146.13(8) . . . . ?
O8 Na2 O6 Na1 -110.41(3) 2_775 . . . ?
Na3 Na2 O6 Na1 126.16(4) . . . . ?
O24 Na2 O1 C1 55.48(15) . . . . ?
O5 Na2 O1 C1 128.18(14) . . . . ?
O6 Na2 O1 C1 163.07(15) . . . . ?
O23 Na2 O1 C1 -29.65(16) . . . . ?
O8 Na2 O1 C1 -109.71(15) 2_775 . . . ?
Na3 Na2 O1 C1 17.11(16) . . . . ?
Na1 Na2 O1 C1 164.11(16) . . . . ?
O24 Na2 O1 Na1 -108.63(3) . . . . ?
O5 Na2 O1 Na1 -35.93(8) . . . . ?
O6 Na2 O1 Na1 -1.04(3) . . . . ?
O23 Na2 O1 Na1 166.24(3) . . . . ?
O8 Na2 O1 Na1 86.18(3) 2_775 . . . ?
Na3 Na2 O1 Na1 -147.00(2) . . . . ?
Na3 O7 C10 C9 -22.98(15) 1_655 . . . ?
Na3 O7 C10 C11 156.54(7) 1_655 . . . ?
Na1 O6 C8 C9 17.1(2) . . . . ?
Na2 O6 C8 C9 -165.01(9) . . . . ?
Na1 O6 C8 C7 -163.45(9) . . . . ?
Na2 O6 C8 C7 14.46(12) . . . . ?
O3 C4 C3 O2 3.10(14) . . . . ?
C5 C4 C3 O2 -177.58(10) . . . . ?
O3 C4 C3 C2 -175.16(10) . . . . ?
C5 C4 C3 C2 4.15(15) . . . . ?
O3 C4 C5 C6 173.91(11) . . . . ?
C3 C4 C5 C6 -5.34(16) . . . . ?
O3 C4 C5 Cl2 -3.18(15) . . . . ?
C3 C4 C5 Cl2 177.57(7) . . . . ?
O7 C10 C9 C8 -175.23(10) . . . . ?
C11 C10 C9 C8 5.25(16) . . . . ?
O7 C10 C9 Cl3 -0.47(15) . . . . ?
C11 C10 C9 Cl3 -179.99(7) . . . . ?
O6 C8 C9 C10 173.55(10) . . . . ?
C7 C8 C9 C10 -5.92(15) . . . . ?
O6 C8 C9 Cl3 -1.26(15) . . . . ?
C7 C8 C9 Cl3 179.27(7) . . . . ?
Na3 Cl3 C9 C10 14.41(9) 1_655 . . . ?
Na3 Cl3 C9 C8 -170.53(8) 1_655 . . . ?
Na1 O4 C6 C5 -163.93(9) . . . . ?
Na1 O4 C6 C1 16.88(12) . . . . ?
C4 C5 C6 O4 -177.23(11) . . . . ?
Cl2 C5 C6 O4 -0.23(16) . . . . ?
C4 C5 C6 C1 1.96(16) . . . . ?
Cl2 C5 C6 C1 178.96(7) . . . . ?
Na2 O8 C11 C12 -98.81(11) 2_775 . . . ?
Na2 O8 C11 C10 80.96(9) 2_775 . . . ?
O7 C10 C11 O8 1.03(14) . . . . ?
C9 C10 C11 O8 -179.42(10) . . . . ?
O7 C10 C11 C12 -179.18(10) . . . . ?
C9 C10 C11 C12 0.37(14) . . . . ?
O8 C11 C12 C7 174.65(10) . . . . ?
C10 C11 C12 C7 -5.12(15) . . . . ?
O8 C11 C12 Cl4 -2.22(15) . . . . ?
C10 C11 C12 Cl4 178.01(7) . . . . ?
Na2 O5 C7 C12 163.40(8) . . . . ?
Na2 O5 C7 C8 -15.78(12) . . . . ?
C11 C12 C7 O5 -174.75(10) . . . . ?
Cl4 C12 C7 O5 2.17(15) . . . . ?
C11 C12 C7 C8 4.40(15) . . . . ?
Cl4 C12 C7 C8 -178.68(7) . . . . ?
O6 C8 C7 O5 0.82(14) . . . . ?
C9 C8 C7 O5 -179.67(10) . . . . ?
O6 C8 C7 C12 -178.41(10) . . . . ?
C9 C8 C7 C12 1.10(14) . . . . ?
O2 C3 C2 C1 -177.71(10) . . . . ?
C4 C3 C2 C1 0.48(16) . . . . ?
O2 C3 C2 Cl1 0.36(15) . . . . ?
C4 C3 C2 Cl1 178.55(8) . . . . ?
Na2 O1 C1 C2 -1.0(2) . . . . ?
Na1 O1 C1 C2 161.32(8) . . . . ?
Na2 O1 C1 C6 178.32(10) . . . . ?
Na1 O1 C1 C6 -19.35(12) . . . . ?
C3 C2 C1 O1 175.44(10) . . . . ?
Cl1 C2 C1 O1 -2.65(15) . . . . ?
C3 C2 C1 C6 -3.89(15) . . . . ?
Cl1 C2 C1 C6 178.03(7) . . . . ?
O4 C6 C1 O1 2.67(15) . . . . ?
C5 C6 C1 O1 -176.60(10) . . . . ?
O4 C6 C1 C2 -177.96(10) . . . . ?
C5 C6 C1 C2 2.77(14) . . . . ?
C8 O6 Na1 O22 95.67(13) . . . . ?
Na2 O6 Na1 O22 -82.46(3) . . . . ?
C8 O6 Na1 O20 -81.28(14) . . . . ?
Na2 O6 Na1 O20 100.59(4) . . . . ?
C8 O6 Na1 O21 5.09(15) . . . . ?
Na2 O6 Na1 O21 -173.04(4) . . . . ?
C8 O6 Na1 O4 -166.44(12) . . . . ?
Na2 O6 Na1 O4 15.44(8) . . . . ?
C8 O6 Na1 O1 177.08(14) . . . . ?
Na2 O6 Na1 O1 -1.05(3) . . . . ?
C8 O6 Na1 Na2 178.13(15) . . . . ?
C6 O4 Na1 O22 57.95(9) . . . . ?
C6 O4 Na1 O20 -122.26(9) . . . . ?
C6 O4 Na1 O21 149.87(9) . . . . ?
C6 O4 Na1 O6 -36.81(12) . . . . ?
C6 O4 Na1 O1 -18.74(8) . . . . ?
C6 O4 Na1 Na2 -26.21(9) . . . . ?
C1 O1 Na1 O22 -82.57(8) . . . . ?
Na2 O1 Na1 O22 88.65(3) . . . . ?
C1 O1 Na1 O20 102.15(8) . . . . ?
Na2 O1 Na1 O20 -86.64(4) . . . . ?
C1 O1 Na1 O21 -2.04(12) . . . . ?
Na2 O1 Na1 O21 169.17(6) . . . . ?
C1 O1 Na1 O6 -170.17(8) . . . . ?
Na2 O1 Na1 O6 1.05(3) . . . . ?
C1 O1 Na1 O4 19.65(7) . . . . ?
Na2 O1 Na1 O4 -169.13(4) . . . . ?
C1 O1 Na1 Na2 -171.22(9) . . . . ?
O1 Na2 Na1 O22 -85.06(4) . . . . ?
O24 Na2 Na1 O22 -7.69(3) . . . . ?
O5 Na2 Na1 O22 76.58(3) . . . . ?
O6 Na2 Na1 O22 93.37(4) . . . . ?
O23 Na2 Na1 O22 -115.67(6) . . . . ?
O8 Na2 Na1 O22 166.88(3) 2_775 . . . ?
Na3 Na2 Na1 O22 -22.14(4) . . . . ?
O1 Na2 Na1 O20 100.11(4) . . . . ?
O24 Na2 Na1 O20 177.49(3) . . . . ?
O5 Na2 Na1 O20 -98.25(4) . . . . ?
O6 Na2 Na1 O20 -81.46(4) . . . . ?
O23 Na2 Na1 O20 69.50(7) . . . . ?
O8 Na2 Na1 O20 -7.95(3) 2_775 . . . ?
Na3 Na2 Na1 O20 163.04(3) . . . . ?
O1 Na2 Na1 O21 -149.50(17) . . . . ?
O24 Na2 Na1 O21 -72.13(17) . . . . ?
O5 Na2 Na1 O21 12.13(17) . . . . ?
O6 Na2 Na1 O21 28.93(17) . . . . ?
O23 Na2 Na1 O21 179.89(16) . . . . ?
O8 Na2 Na1 O21 102.43(17) 2_775 . . . ?
Na3 Na2 Na1 O21 -86.58(17) . . . . ?
O1 Na2 Na1 O6 -178.43(5) . . . . ?
O24 Na2 Na1 O6 -101.06(4) . . . . ?
O5 Na2 Na1 O6 -16.80(4) . . . . ?
O23 Na2 Na1 O6 150.96(7) . . . . ?
O8 Na2 Na1 O6 73.50(4) 2_775 . . . ?
Na3 Na2 Na1 O6 -115.51(5) . . . . ?
O1 Na2 Na1 O4 10.26(4) . . . . ?
O24 Na2 Na1 O4 87.64(4) . . . . ?
O5 Na2 Na1 O4 171.90(3) . . . . ?
O6 Na2 Na1 O4 -171.30(4) . . . . ?
O23 Na2 Na1 O4 -20.34(7) . . . . ?
O8 Na2 Na1 O4 -97.80(3) 2_775 . . . ?
Na3 Na2 Na1 O4 73.19(4) . . . . ?
O24 Na2 Na1 O1 77.38(4) . . . . ?
O5 Na2 Na1 O1 161.64(4) . . . . ?
O6 Na2 Na1 O1 178.43(5) . . . . ?
O23 Na2 Na1 O1 -30.61(6) . . . . ?
O8 Na2 Na1 O1 -108.06(4) 2_775 . . . ?
Na3 Na2 Na1 O1 62.92(4) . . . . ?
Na2 O24 Na3 O26 -168.06(3) . . . . ?
Na2 O24 Na3 O7 -140.81(17) . . . 1_455 ?
Na2 O24 Na3 O23 13.49(3) . . . . ?
Na2 O24 Na3 O25 -77.75(3) . . . . ?
Na2 O24 Na3 Cl3 103.45(3) . . . 1_455 ?
Na2 O24 Na3 Na4 -122.71(3) . . . . ?
Na4 O25 Na3 O26 1.02(3) . . . . ?
Na4 O25 Na3 O7 84.89(3) . . . 1_455 ?
Na4 O25 Na3 O23 -172.69(3) . . . . ?
Na4 O25 Na3 O24 -85.17(3) . . . . ?
Na4 O25 Na3 Cl3 92.60(6) . . . 1_455 ?
Na4 O25 Na3 Na2 -127.46(3) . . . . ?
O1 Na2 Na3 O26 79.49(4) . . . . ?
O24 Na2 Na3 O26 15.19(4) . . . . ?
O5 Na2 Na3 O26 -71.58(4) . . . . ?
O6 Na2 Na3 O26 -37.30(6) . . . . ?
O23 Na2 Na3 O26 176.34(5) . . . . ?
O8 Na2 Na3 O26 -153.68(4) 2_775 . . . ?
Na1 Na2 Na3 O26 35.78(5) . . . . ?
O1 Na2 Na3 O7 -128.03(5) . . . 1_455 ?
O24 Na2 Na3 O7 167.67(6) . . . 1_455 ?
O5 Na2 Na3 O7 80.91(5) . . . 1_455 ?
O6 Na2 Na3 O7 115.18(6) . . . 1_455 ?
O23 Na2 Na3 O7 -31.17(5) . . . 1_455 ?
O8 Na2 Na3 O7 -1.19(6) 2_775 . . 1_455 ?
Na1 Na2 Na3 O7 -171.73(4) . . . 1_455 ?
O1 Na2 Na3 O23 -96.85(4) . . . . ?
O24 Na2 Na3 O23 -161.15(5) . . . . ?
O5 Na2 Na3 O23 112.08(4) . . . . ?
O6 Na2 Na3 O23 146.35(5) . . . . ?
O8 Na2 Na3 O23 29.98(4) 2_775 . . . ?
Na1 Na2 Na3 O23 -140.56(4) . . . . ?
O1 Na2 Na3 O24 64.30(4) . . . . ?
O5 Na2 Na3 O24 -86.77(4) . . . . ?
O6 Na2 Na3 O24 -52.49(5) . . . . ?
O23 Na2 Na3 O24 161.15(5) . . . . ?
O8 Na2 Na3 O24 -168.86(4) 2_775 . . . ?
Na1 Na2 Na3 O24 20.60(4) . . . . ?
O1 Na2 Na3 O25 162.97(4) . . . . ?
O24 Na2 Na3 O25 98.67(4) . . . . ?
O5 Na2 Na3 O25 11.91(3) . . . . ?
O6 Na2 Na3 O25 46.18(5) . . . . ?
O23 Na2 Na3 O25 -100.17(4) . . . . ?
O8 Na2 Na3 O25 -70.19(3) 2_775 . . . ?
Na1 Na2 Na3 O25 119.27(4) . . . . ?
O1 Na2 Na3 Cl3 -37.34(3) . . . 1_455 ?
O24 Na2 Na3 Cl3 -101.64(4) . . . 1_455 ?
O5 Na2 Na3 Cl3 171.59(3) . . . 1_455 ?
O6 Na2 Na3 Cl3 -154.14(4) . . . 1_455 ?
O23 Na2 Na3 Cl3 59.51(3) . . . 1_455 ?
O8 Na2 Na3 Cl3 89.49(3) 2_775 . . 1_455 ?
Na1 Na2 Na3 Cl3 -81.05(3) . . . 1_455 ?
O1 Na2 Na3 Na4 126.63(3) . . . . ?
O24 Na2 Na3 Na4 62.34(3) . . . . ?
O5 Na2 Na3 Na4 -24.43(3) . . . . ?
O6 Na2 Na3 Na4 9.84(5) . . . . ?
O23 Na2 Na3 Na4 -136.51(4) . . . . ?
O8 Na2 Na3 Na4 -106.53(3) 2_775 . . . ?
Na1 Na2 Na3 Na4 82.93(3) . . . . ?
C13 O9 Na4 O27 -143.2(11) . . . . ?
C13 O9 Na4 O25 70.03(10) . . . . ?
C13 O9 Na4 O28 -112.63(11) . . . . ?
C13 O9 Na4 O26 159.39(10) . . . . ?
C13 O9 Na4 Cl6 -26.51(9) . . . . ?
C13 O9 Na4 Na3 115.60(10) . . . . ?
C13 O9 Na4 Na5 -121.08(10) . . . . ?
Na3 O25 Na4 O9 88.08(3) . . . . ?
Na3 O25 Na4 O27 -90.85(3) . . . . ?
Na3 O25 Na4 O28 -68.3(4) . . . . ?
Na3 O25 Na4 O26 -0.99(3) . . . . ?
Na3 O25 Na4 Cl6 151.80(2) . . . . ?
Na3 O25 Na4 Na5 -81.59(4) . . . . ?
C18 Cl6 Na4 O9 16.81(4) . . . . ?
C18 Cl6 Na4 O27 -165.15(5) . . . . ?
C18 Cl6 Na4 O25 -70.64(4) . . . . ?
C18 Cl6 Na4 O28 113.62(5) . . . . ?
C18 Cl6 Na4 O26 29.60(7) . . . . ?
C18 Cl6 Na4 Na3 -42.45(4) . . . . ?
C18 Cl6 Na4 Na5 149.11(4) . . . . ?
O26 Na3 Na4 O9 89.81(4) . . . . ?
O7 Na3 Na4 O9 177.95(3) 1_455 . . . ?
O23 Na3 Na4 O9 -81.12(5) . . . . ?
O24 Na3 Na4 O9 1.42(3) . . . . ?
O25 Na3 Na4 O9 -91.62(4) . . . . ?
Cl3 Na3 Na4 O9 126.02(3) 1_455 . . . ?
Na2 Na3 Na4 O9 -35.75(3) . . . . ?
O26 Na3 Na4 O27 -88.26(4) . . . . ?
O7 Na3 Na4 O27 -0.12(3) 1_455 . . . ?
O23 Na3 Na4 O27 100.81(4) . . . . ?
O24 Na3 Na4 O27 -176.66(3) . . . . ?
O25 Na3 Na4 O27 90.30(4) . . . . ?
Cl3 Na3 Na4 O27 -52.06(3) 1_455 . . . ?
Na2 Na3 Na4 O27 146.17(3) . . . . ?
O26 Na3 Na4 O25 -178.56(5) . . . . ?
O7 Na3 Na4 O25 -90.42(4) 1_455 . . . ?
O23 Na3 Na4 O25 10.51(5) . . . . ?
O24 Na3 Na4 O25 93.04(4) . . . . ?
Cl3 Na3 Na4 O25 -142.36(4) 1_455 . . . ?
Na2 Na3 Na4 O25 55.87(3) . . . . ?
O26 Na3 Na4 O28 -6.82(5) . . . . ?
O7 Na3 Na4 O28 81.32(4) 1_455 . . . ?
O23 Na3 Na4 O28 -177.75(5) . . . . ?
O24 Na3 Na4 O28 -95.21(4) . . . . ?
O25 Na3 Na4 O28 171.75(5) . . . . ?
Cl3 Na3 Na4 O28 29.39(5) 1_455 . . . ?
Na2 Na3 Na4 O28 -132.38(4) . . . . ?
O7 Na3 Na4 O26 88.14(4) 1_455 . . . ?
O23 Na3 Na4 O26 -170.93(5) . . . . ?
O24 Na3 Na4 O26 -88.40(4) . . . . ?
O25 Na3 Na4 O26 178.56(5) . . . . ?
Cl3 Na3 Na4 O26 36.21(4) 1_455 . . . ?
Na2 Na3 Na4 O26 -125.57(4) . . . . ?
O26 Na3 Na4 Cl6 140.30(4) . . . . ?
O7 Na3 Na4 Cl6 -131.55(3) 1_455 . . . ?
O23 Na3 Na4 Cl6 -30.62(5) . . . . ?
O24 Na3 Na4 Cl6 51.91(3) . . . . ?
O25 Na3 Na4 Cl6 -41.13(4) . . . . ?
Cl3 Na3 Na4 Cl6 176.512(19) 1_455 . . . ?
Na2 Na3 Na4 Cl6 14.74(3) . . . . ?
O26 Na3 Na4 Na5 -51.37(3) . . . . ?
O7 Na3 Na4 Na5 36.77(3) 1_455 . . . ?
O23 Na3 Na4 Na5 137.70(4) . . . . ?
O24 Na3 Na4 Na5 -139.77(3) . . . . ?
O25 Na3 Na4 Na5 127.19(3) . . . . ?
Cl3 Na3 Na4 Na5 -15.17(3) 1_455 . . . ?
Na2 Na3 Na4 Na5 -176.940(16) . . . . ?
O12 Na5 Na4 O9 124.23(5) 2_685 . . . ?
O28 Na5 Na4 O9 12.78(6) . . . . ?
O12 Na5 Na4 O9 -127.61(5) 1_455 . . . ?
O27 Na5 Na4 O9 -178.89(5) . . . . ?
O11 Na5 Na4 O9 -86.94(5) 1_455 . . . ?
O29 Na5 Na4 O9 4.86(5) . . . . ?
Na5 Na5 Na4 O9 169.93(4) 2_585 . . . ?
O12 Na5 Na4 O27 -56.88(4) 2_685 . . . ?
O28 Na5 Na4 O27 -168.33(6) . . . . ?
O12 Na5 Na4 O27 51.28(5) 1_455 . . . ?
O11 Na5 Na4 O27 91.95(4) 1_455 . . . ?
O29 Na5 Na4 O27 -176.25(5) . . . . ?
Na5 Na5 Na4 O27 -11.18(4) 2_585 . . . ?
O12 Na5 Na4 O25 -70.85(5) 2_685 . . . ?
O28 Na5 Na4 O25 177.70(6) . . . . ?
O12 Na5 Na4 O25 37.31(6) 1_455 . . . ?
O27 Na5 Na4 O25 -13.97(5) . . . . ?
O11 Na5 Na4 O25 77.98(4) 1_455 . . . ?
O29 Na5 Na4 O25 169.78(4) . . . . ?
Na5 Na5 Na4 O25 -25.15(6) 2_585 . . . ?
O12 Na5 Na4 O28 111.45(6) 2_685 . . . ?
O12 Na5 Na4 O28 -140.39(6) 1_455 . . . ?
O27 Na5 Na4 O28 168.33(6) . . . . ?
O11 Na5 Na4 O28 -99.72(6) 1_455 . . . ?
O29 Na5 Na4 O28 -7.92(6) . . . . ?
Na5 Na5 Na4 O28 157.15(6) 2_585 . . . ?
O12 Na5 Na4 O26 -154.03(4) 2_685 . . . ?
O28 Na5 Na4 O26 94.52(6) . . . . ?
O12 Na5 Na4 O26 -45.87(4) 1_455 . . . ?
O27 Na5 Na4 O26 -97.15(4) . . . . ?
O11 Na5 Na4 O26 -5.20(3) 1_455 . . . ?
O29 Na5 Na4 O26 86.60(4) . . . . ?
Na5 Na5 Na4 O26 -108.33(4) 2_585 . . . ?
O12 Na5 Na4 Cl6 49.99(3) 2_685 . . . ?
O28 Na5 Na4 Cl6 -61.47(5) . . . . ?
O12 Na5 Na4 Cl6 158.15(3) 1_455 . . . ?
O27 Na5 Na4 Cl6 106.87(4) . . . . ?
O11 Na5 Na4 Cl6 -161.18(3) 1_455 . . . ?
O29 Na5 Na4 Cl6 -69.38(3) . . . . ?
Na5 Na5 Na4 Cl6 95.68(3) 2_585 . . . ?
O12 Na5 Na4 Na3 -121.06(3) 2_685 . . . ?
O28 Na5 Na4 Na3 127.49(5) . . . . ?
O12 Na5 Na4 Na3 -12.90(4) 1_455 . . . ?
O27 Na5 Na4 Na3 -64.18(3) . . . . ?
O11 Na5 Na4 Na3 27.77(3) 1_455 . . . ?
O29 Na5 Na4 Na3 119.57(3) . . . . ?
Na5 Na5 Na4 Na3 -75.37(4) 2_585 . . . ?
O9 Na4 O27 Na5 23.0(11) . . . . ?
O25 Na4 O27 Na5 169.70(3) . . . . ?
O28 Na4 O27 Na5 -7.74(4) . . . . ?
O26 Na4 O27 Na5 80.33(3) . . . . ?
Cl6 Na4 O27 Na5 -92.87(3) . . . . ?
Na3 Na4 O27 Na5 124.10(3) . . . . ?
O12 Na5 O27 Na4 130.51(3) 2_685 . . . ?
O28 Na5 O27 Na4 7.80(4) . . . . ?
O12 Na5 O27 Na4 -145.22(3) 1_455 . . . ?
O11 Na5 O27 Na4 -81.02(3) 1_455 . . . ?
O29 Na5 O27 Na4 13.92(17) . . . . ?
Na5 Na5 O27 Na4 172.70(3) 2_585 . . . ?
O7 Na3 O26 Na4 -86.47(3) 1_455 . . . ?
O23 Na3 O26 Na4 102.3(3) . . . . ?
O24 Na3 O26 Na4 88.43(3) . . . . ?
O25 Na3 O26 Na4 -1.02(3) . . . . ?
Cl3 Na3 O26 Na4 -152.96(3) 1_455 . . . ?
Na2 Na3 O26 Na4 78.13(4) . . . . ?
O9 Na4 O26 Na3 -89.37(3) . . . . ?
O27 Na4 O26 Na3 92.28(3) . . . . ?
O25 Na4 O26 Na3 1.03(3) . . . . ?
O28 Na4 O26 Na3 174.91(4) . . . . ?
Cl6 Na4 O26 Na3 -100.84(6) . . . . ?
Na5 Na4 O26 Na3 133.69(3) . . . . ?
O26 Na3 O23 Na2 -26.5(3) . . . . ?
O7 Na3 O23 Na2 162.37(3) 1_455 . . . ?
O24 Na3 O23 Na2 -12.72(3) . . . . ?
O25 Na3 O23 Na2 76.69(3) . . . . ?
Cl3 Na3 O23 Na2 -131.27(2) 1_455 . . . ?
Na4 Na3 O23 Na2 69.28(4) . . . . ?
O1 Na2 O23 Na3 102.05(4) . . . . ?
O24 Na2 O23 Na3 12.91(3) . . . . ?
O5 Na2 O23 Na3 -66.77(3) . . . . ?
O6 Na2 O23 Na3 -113.47(9) . . . . ?
O8 Na2 O23 Na3 -150.97(3) 2_775 . . . ?
Na1 Na2 O23 Na3 124.95(5) . . . . ?
O12 Na5 O28 Na4 -92.04(5) 2_685 . . . ?
O12 Na5 O28 Na4 97.71(8) 1_455 . . . ?
O27 Na5 O28 Na4 -7.62(4) . . . . ?
O11 Na5 O28 Na4 75.15(5) 1_455 . . . ?
O29 Na5 O28 Na4 173.70(5) . . . . ?
Na5 Na5 O28 Na4 -103.89(13) 2_585 . . . ?
O9 Na4 O28 Na5 -171.18(4) . . . . ?
O27 Na4 O28 Na5 7.81(4) . . . . ?
O25 Na4 O28 Na5 -14.9(4) . . . . ?
O26 Na4 O28 Na5 -82.30(4) . . . . ?
Cl6 Na4 O28 Na5 125.23(4) . . . . ?
Na3 Na4 O28 Na5 -77.59(5) . . . . ?

data_RbHCA(H2O)2
_database_code_depnum_ccdc_archive 'CCDC 669456'

_audit_creation_date             2007-08-23T09:38:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C6 H5 Cl2 O6 Rb1'
_chemical_formula_sum            'C6 H5 Cl2 O6 Rb'
_chemical_formula_weight         329.47

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
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                   9.134(5)
_cell_length_b                   6.923(5)
_cell_length_c                   15.844(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 94.092(5)
_cell_angle_gamma                90.000
_cell_volume                     999.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      8
_cell_measurement_theta_max      19.7

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_diffrn    2.19
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    11.866
_exptl_absorpt_correction_type   none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        2
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 2 0
1 2 -3
3 1 -2

_diffrn_reflns_number            2222
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         5.43
_diffrn_reflns_theta_max         76.18
_diffrn_reflns_theta_full        76.18
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_reflns_number_total             2092
_reflns_number_gt                2032
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_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)+(0.0977P)²+1.4842P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.087(6)
_refine_ls_number_reflns         2092
_refine_ls_number_parameters     157
_refine_ls_number_restraints     7
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1361
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.008
_refine_diff_density_max         1.275
_refine_diff_density_min         -1.401

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Rb1 Rb 0.53727(4) -0.02937(7) 0.35499(3) 0.0416(3) Uani 1 d . . .
Cl2 Cl 1.13706(9) 0.24352(12) 0.36205(5) 0.0281(3) Uani 1 d . . .
Cl1 Cl 0.80087(10) 0.25640(14) 0.69608(5) 0.0351(3) Uani 1 d . . .
C2 C 0.8918(4) 0.2531(5) 0.6049(2) 0.0241(7) Uani 1 d . . .
O4 O 0.8305(3) 0.1137(4) 0.38222(16) 0.0329(6) Uani 1 d . . .
O1 O 0.6863(3) 0.1352(4) 0.52404(16) 0.0342(6) Uani 1 d . . .
O2 O 1.1055(3) 0.3670(4) 0.67736(15) 0.0314(6) Uani 1 d D . .
C1 C 0.8139(3) 0.1864(5) 0.5279(2) 0.0233(6) Uani 1 d . . .
O3 O 1.2471(3) 0.3653(5) 0.53528(16) 0.0337(6) Uani 1 d . . .
C3 C 1.0340(4) 0.3086(5) 0.60680(19) 0.0222(6) Uani 1 d . . .
C5 C 1.0430(4) 0.2439(4) 0.4525(2) 0.0222(6) Uani 1 d . . .
O5 O 0.4770(4) 0.3739(6) 0.4096(2) 0.0512(8) Uani 1 d D . .
C4 C 1.1178(3) 0.3078(5) 0.5276(2) 0.0220(6) Uani 1 d . . .
C6 C 0.8976(4) 0.1784(5) 0.44671(19) 0.0224(6) Uani 1 d . . .
O6 O 0.6163(3) -0.4089(6) 0.28949(18) 0.0439(7) Uani 1 d D . .
H6B H 0.670(13) -0.512(11) 0.316(5) 0.14(5) Uiso 1 d D . .
H6A H 0.605(10) -0.445(12) 0.2317(19) 0.10(3) Uiso 1 d D . .
H5A H 0.541(6) 0.350(13) 0.457(3) 0.09(2) Uiso 1 d D . .
H5B H 0.382(4) 0.38(2) 0.428(5) 0.15(4) Uiso 1 d D . .
H H 1.12(3) 0.482(12) 0.661(15) 0.30(13) Uiso 1 d D . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
Rb1 O4 2.859(3) . ?
Rb1 O6 2.934(4) . ?
Rb1 O5 2.986(5) . ?
Rb1 O1 2.990(3) 3_656 ?
Rb1 O1 3.131(3) . ?
Rb1 O2 3.134(3) 4_565 ?
Rb1 O3 3.438(3) 3_756 ?
Rb1 Cl1 3.5083(18) 3_656 ?
Rb1 Cl1 3.7145(15) 4_565 ?
Rb1 Rb1 4.7106(16) 3_656 ?
Rb1 H5A 3.09(8) . ?
Cl2 C5 1.723(3) . ?
Cl1 C2 1.717(3) . ?
Cl1 Rb1 3.5083(18) 3_656 ?
Cl1 Rb1 3.7145(15) 4_666 ?
C2 C3 1.352(5) . ?
C2 C1 1.445(4) . ?
O4 C6 1.237(4) . ?
O1 C1 1.216(4) . ?
O1 Rb1 2.990(3) 3_656 ?
O2 C3 1.317(4) . ?
O2 Rb1 3.134(3) 4_666 ?
O2 H 0.85(12) . ?
C1 C6 1.543(4) . ?
O3 C4 1.243(4) . ?
O3 Rb1 3.438(3) 3_756 ?
C3 C4 1.516(4) . ?
C5 C6 1.400(5) . ?
C5 C4 1.401(5) . ?
O5 H5A 0.94(2) . ?
O5 H5B 0.94(2) . ?
O6 H6B 0.95(9) . ?
O6 H6A 0.95(2) . ?

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
O4 Rb1 O6 96.45(9) . . ?
O4 Rb1 O5 79.77(9) . . ?
O6 Rb1 O5 174.27(9) . . ?
O4 Rb1 O1 131.56(7) . 3_656 ?
O6 Rb1 O1 101.75(9) . 3_656 ?
O5 Rb1 O1 83.97(9) . 3_656 ?
O4 Rb1 O1 53.10(7) . . ?
O6 Rb1 O1 121.70(8) . . ?
O5 Rb1 O1 59.31(9) . . ?
O1 Rb1 O1 79.39(8) 3_656 . ?
O4 Rb1 O2 76.53(7) . 4_565 ?
O6 Rb1 O2 86.22(9) . 4_565 ?
O5 Rb1 O2 88.71(9) . 4_565 ?
O1 Rb1 O2 148.45(7) 3_656 4_565 ?
O1 Rb1 O2 122.37(8) . 4_565 ?
O4 Rb1 O3 70.21(8) . 3_756 ?
O6 Rb1 O3 55.01(8) . 3_756 ?
O5 Rb1 O3 126.63(8) . 3_756 ?
O1 Rb1 O3 84.43(8) 3_656 3_756 ?
O1 Rb1 O3 67.37(8) . 3_756 ?
O2 Rb1 O3 123.59(7) 4_565 3_756 ?
O4 Rb1 Cl1 171.79(6) . 3_656 ?
O6 Rb1 Cl1 75.64(7) . 3_656 ?
O5 Rb1 Cl1 107.96(7) . 3_656 ?
O1 Rb1 Cl1 53.68(6) 3_656 3_656 ?
O1 Rb1 Cl1 133.01(5) . 3_656 ?
O2 Rb1 Cl1 100.47(6) 4_565 3_656 ?
O3 Rb1 Cl1 106.07(6) 3_756 3_656 ?
O4 Rb1 Cl1 114.77(7) . 4_565 ?
O6 Rb1 Cl1 111.20(7) . 4_565 ?
O5 Rb1 Cl1 67.08(7) . 4_565 ?
O1 Rb1 Cl1 99.71(7) 3_656 4_565 ?
O1 Rb1 Cl1 126.22(7) . 4_565 ?
O2 Rb1 Cl1 49.61(5) 4_565 4_565 ?
O3 Rb1 Cl1 166.21(5) 3_756 4_565 ?
Cl1 Rb1 Cl1 67.17(4) 3_656 4_565 ?
O4 Rb1 Rb1 91.26(5) . 3_656 ?
O6 Rb1 Rb1 118.60(6) . 3_656 ?
O5 Rb1 Rb1 66.05(7) . 3_656 ?
O1 Rb1 Rb1 40.80(5) 3_656 3_656 ?
O1 Rb1 Rb1 38.60(5) . 3_656 ?
O2 Rb1 Rb1 153.74(6) 4_565 3_656 ?
O3 Rb1 Rb1 71.49(5) 3_756 3_656 ?
Cl1 Rb1 Rb1 94.44(2) 3_656 3_656 ?
Cl1 Rb1 Rb1 119.99(3) 4_565 3_656 ?
O4 Rb1 H5A 69.5(11) . . ?
O6 Rb1 H5A 162.6(6) . . ?
O5 Rb1 H5A 17.7(5) . . ?
O1 Rb1 H5A 81.7(14) 3_656 . ?
O1 Rb1 H5A 41.7(6) . . ?
O2 Rb1 H5A 99.8(12) 4_565 . ?
O3 Rb1 H5A 109.0(6) 3_756 . ?
Cl1 Rb1 H5A 118.7(11) 3_656 . ?
Cl1 Rb1 H5A 84.7(6) 4_565 . ?
Rb1 Rb1 H5A 54.0(12) 3_656 . ?
C2 Cl1 Rb1 105.72(12) . 3_656 ?
C2 Cl1 Rb1 106.51(12) . 4_666 ?
Rb1 Cl1 Rb1 147.55(3) 3_656 4_666 ?
C3 C2 C1 121.6(3) . . ?
C3 C2 Cl1 119.9(3) . . ?
C1 C2 Cl1 118.4(2) . . ?
C6 O4 Rb1 130.8(2) . . ?
C1 O1 Rb1 137.4(2) . 3_656 ?
C1 O1 Rb1 120.4(2) . . ?
Rb1 O1 Rb1 100.61(8) 3_656 . ?
C3 O2 Rb1 138.9(2) . 4_666 ?
C3 O2 H 95(10) . . ?
Rb1 O2 H 89(10) 4_666 . ?
O1 C1 C2 123.2(3) . . ?
O1 C1 C6 118.6(3) . . ?
C2 C1 C6 118.2(3) . . ?
C4 O3 Rb1 109.8(2) . 3_756 ?
O2 C3 C2 121.5(3) . . ?
O2 C3 C4 117.0(3) . . ?
C2 C3 C4 121.4(3) . . ?
C6 C5 C4 124.1(3) . . ?
C6 C5 Cl2 118.2(2) . . ?
C4 C5 Cl2 117.7(2) . . ?
Rb1 O5 H5A 87(5) . . ?
Rb1 O5 H5B 111(9) . . ?
H5A O5 H5B 108(4) . . ?
O3 C4 C5 125.9(3) . . ?
O3 C4 C3 116.8(3) . . ?
C5 C4 C3 117.3(3) . . ?
O4 C6 C5 125.7(3) . . ?
O4 C6 C1 117.1(3) . . ?
C5 C6 C1 117.2(3) . . ?
Rb1 O6 H6B 130(6) . . ?
Rb1 O6 H6A 125(5) . . ?
H6B O6 H6A 104(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rb1 Cl1 C2 C3 -171.6(2) 3_656 . . . ?
Rb1 Cl1 C2 C3 12.2(3) 4_666 . . . ?
Rb1 Cl1 C2 C1 7.1(3) 3_656 . . . ?
Rb1 Cl1 C2 C1 -169.1(2) 4_666 . . . ?
O6 Rb1 O4 C6 -124.2(3) . . . . ?
O5 Rb1 O4 C6 60.1(3) . . . . ?
O1 Rb1 O4 C6 -12.2(4) 3_656 . . . ?
O1 Rb1 O4 C6 1.0(3) . . . . ?
O2 Rb1 O4 C6 151.3(3) 4_565 . . . ?
O3 Rb1 O4 C6 -75.0(3) 3_756 . . . ?
Cl1 Rb1 O4 C6 -139.3(3) 3_656 . . . ?
Cl1 Rb1 O4 C6 118.9(3) 4_565 . . . ?
Rb1 Rb1 O4 C6 -5.2(3) 3_656 . . . ?
O4 Rb1 O1 C1 -2.2(3) . . . . ?
O6 Rb1 O1 C1 70.4(3) . . . . ?
O5 Rb1 O1 C1 -103.0(3) . . . . ?
O1 Rb1 O1 C1 167.8(3) 3_656 . . . ?
O2 Rb1 O1 C1 -37.0(3) 4_565 . . . ?
O3 Rb1 O1 C1 79.4(3) 3_756 . . . ?
Cl1 Rb1 O1 C1 170.6(2) 3_656 . . . ?
Cl1 Rb1 O1 C1 -97.9(3) 4_565 . . . ?
Rb1 Rb1 O1 C1 167.8(3) 3_656 . . . ?
O4 Rb1 O1 Rb1 -169.97(14) . . . 3_656 ?
O6 Rb1 O1 Rb1 -97.35(11) . . . 3_656 ?
O5 Rb1 O1 Rb1 89.24(11) . . . 3_656 ?
O1 Rb1 O1 Rb1 0 3_656 . . 3_656 ?
O2 Rb1 O1 Rb1 155.21(8) 4_565 . . 3_656 ?
O3 Rb1 O1 Rb1 -88.34(9) 3_756 . . 3_656 ?
Cl1 Rb1 O1 Rb1 2.87(13) 3_656 . . 3_656 ?
Cl1 Rb1 O1 Rb1 94.33(9) 4_565 . . 3_656 ?
Rb1 O1 C1 C2 -14.2(6) 3_656 . . . ?
Rb1 O1 C1 C2 -176.3(2) . . . . ?
Rb1 O1 C1 C6 165.2(2) 3_656 . . . ?
Rb1 O1 C1 C6 3.2(4) . . . . ?
C3 C2 C1 O1 179.9(3) . . . . ?
Cl1 C2 C1 O1 1.2(5) . . . . ?
C3 C2 C1 C6 0.4(5) . . . . ?
Cl1 C2 C1 C6 -178.3(2) . . . . ?
Rb1 O2 C3 C2 -20.5(5) 4_666 . . . ?
Rb1 O2 C3 C4 159.0(2) 4_666 . . . ?
C1 C2 C3 O2 -179.1(3) . . . . ?
Cl1 C2 C3 O2 -0.4(5) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
Cl1 C2 C3 C4 -180.0(2) . . . . ?
Rb1 O3 C4 C5 -108.7(3) 3_756 . . . ?
Rb1 O3 C4 C3 71.7(3) 3_756 . . . ?
C6 C5 C4 O3 179.3(3) . . . . ?
Cl2 C5 C4 O3 0.2(5) . . . . ?
C6 C5 C4 C3 -1.1(5) . . . . ?
Cl2 C5 C4 C3 179.7(2) . . . . ?
O2 C3 C4 O3 -1.1(5) . . . . ?
C2 C3 C4 O3 178.5(3) . . . . ?
O2 C3 C4 C5 179.3(3) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
Rb1 O4 C6 C5 179.6(2) . . . . ?
Rb1 O4 C6 C1 0.0(5) . . . . ?
C4 C5 C6 O4 -176.8(3) . . . . ?
Cl2 C5 C6 O4 2.3(5) . . . . ?
C4 C5 C6 C1 2.8(5) . . . . ?
Cl2 C5 C6 C1 -178.0(2) . . . . ?
O1 C1 C6 O4 -2.2(5) . . . . ?
C2 C1 C6 O4 177.3(3) . . . . ?
O1 C1 C6 C5 178.1(3) . . . . ?
C2 C1 C6 C5 -2.4(4) . . . . ?

