# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_cs2dhq-1
_database_code_depnum_ccdc_archive 'CCDC 889125'
#TrackingRef 'Cs-DHQ-cifdoc.cif'


_audit_creation_date             2010-05-13T13:25:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_moiety         'C6 H2 Cs2 O4'
_chemical_formula_sum            'C6 H2 Cs2 O4'
_chemical_formula_weight         403.89

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

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

_cell_length_a                   8.2553(11)
_cell_length_b                   12.8490(16)
_cell_length_c                   3.8880(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     412.41(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1042
_cell_measurement_theta_min      6.3675
_cell_measurement_theta_max      75.9936

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

_exptl_crystal_description       prism
_exptl_crystal_colour            'orange brown'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    3.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             360
_exptl_absorpt_coefficient_mu    68.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.13266
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54179
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_reflns_number            1318
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         6.37
_diffrn_reflns_theta_max         76.18
_diffrn_reflns_theta_full        76.18
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.986
_reflns_number_total             274
_reflns_number_gt                253
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_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/[\s^2^(Fo^2^)+(0.1252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_number_reflns         274
_refine_ls_number_parameters     25
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.055
_refine_ls_wR_factor_ref         0.1534
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0
_refine_diff_density_max         2.168
_refine_diff_density_min         -1.912

#------------------ 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'
Cs Cs -0.746 7.905 '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
O1 O 0.1755(19) 0 0.5 0.031(3) Uani 1 d S . .
C2 C 0.4137(12) 0.1000(7) 0.5 0.0257(19) Uani 1 d S . .
C1 C 0.3233(17) 0 0.5 0.025(2) Uani 1 d S . .
O2 O 0.331(3) 0.1820(16) 0.5 0.035(4) Uani 0.5 d SP . .
Cs1 Cs 0 0.15737(5) 0 0.0329(6) Uani 1 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.027(7) 0.032(6) 0.035(8) 0 0 0
C2 0.025(5) 0.025(4) 0.027(5) 0 0 0.002(3)
C1 0.016(6) 0.030(5) 0.027(6) 0 0 0
O2 0.046(12) 0.026(7) 0.032(9) 0 0 -0.004(9)
Cs1 0.0396(9) 0.0287(8) 0.0303(8) 0 0 0


#------------------ 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
O1 C1 1.22(2) . ?
C2 O2 1.25(2) . ?
C2 C2 1.43(2) 11_655 ?
C2 C1 1.486(11) . ?
C1 C2 1.486(11) 3_556 ?

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
O2 C2 C2 122.8(11) . 11_655 ?
O2 C2 C1 117.1(13) . . ?
C2 C2 C1 120.1(6) 11_655 . ?
O1 C1 C2 120.1(6) . . ?
O1 C1 C2 120.1(6) . 3_556 ?
C2 C1 C2 119.7(12) . 3_556 ?

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
O2 C2 C1 O1 0 . . . . ?
C2 C2 C1 O1 180 11_655 . . . ?
O2 C2 C1 C2 180 . . . 3_556 ?
C2 C2 C1 C2 0 11_655 . . 3_556 ?


data_k2dhq-1
_database_code_depnum_ccdc_archive 'CCDC 889126'
#TrackingRef 'K2DHQ-cifdoc.cif'


_audit_creation_date             2010-05-13T13:35:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_moiety         'C6 H2 K2 O4'
_chemical_formula_sum            'C6 H2 K2 O4'
_chemical_formula_weight         216.28

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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                   3.92510(10)
_cell_length_b                   11.2358(3)
_cell_length_c                   8.3337(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.757(3)
_cell_angle_gamma                90
_cell_volume                     358.457(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             216
_exptl_absorpt_coefficient_mu    11.47
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54179
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_number            2524
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         6.72
_diffrn_reflns_theta_max         76.09
_diffrn_reflns_theta_full        76.09
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_reflns_number_total             737
_reflns_number_gt                700
_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/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_number_reflns         737
_refine_ls_number_parameters     59
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0845
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.274

#------------------ 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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
H3 H -0.674(7) 0.649(2) 0.675(3) 0.032(6) Uiso 1 d . . .
K1 K 0.23822(8) 0.33603(3) 0.95986(4) 0.0268(2) Uani 1 d . . .
O2 O -0.8627(4) 0.69452(11) 0.36690(16) 0.0311(3) Uani 1 d . . .
O1 O -0.3187(3) 0.47323(10) 0.82939(14) 0.0279(3) Uani 1 d . . .
C3 C -0.5976(4) 0.58959(14) 0.6056(2) 0.0243(4) Uani 1 d . . .
C1 C -0.4070(4) 0.49028(13) 0.67745(18) 0.0207(3) Uani 1 d . . .
C2 C -0.6978(4) 0.60547(13) 0.4353(2) 0.0216(3) Uani 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0300(3) 0.0216(3) 0.0272(3) 0.00276(10) 0.00252(18) 0.00085(10)
O2 0.0439(7) 0.0213(5) 0.0254(6) 0.0017(5) 0.0018(5) 0.0099(5)
O1 0.0365(7) 0.0278(6) 0.0177(6) 0.0015(4) 0.0026(4) 0.0040(4)
C3 0.0322(8) 0.0191(7) 0.0206(7) -0.0029(6) 0.0040(6) 0.0039(6)
C1 0.0246(7) 0.0188(6) 0.0182(7) 0.0000(5) 0.0036(5) -0.0026(5)
C2 0.0258(7) 0.0150(6) 0.0226(7) -0.0002(5) 0.0022(6) 0.0006(5)


#------------------ 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 O1 2.6995(12) . ?
K1 O1 2.7236(13) 1_655 ?
K1 O1 2.7445(12) 3_567 ?
K1 O2 2.7794(13) 2_446 ?
K1 O2 2.8166(13) 3_466 ?
K1 O2 3.0096(14) 2_546 ?
K1 C2 3.1674(14) 2_546 ?
K1 C3 3.2086(16) 2_546 ?
K1 C1 3.4538(15) 1_655 ?
K1 C1 3.5107(16) . ?
K1 C1 3.5354(15) 3_567 ?
K1 K1 3.9251 1_655 ?
O2 C2 1.258(2) . ?
O2 K1 2.7794(13) 2_456 ?
O2 K1 2.8166(13) 3_466 ?
O2 K1 3.0096(14) 2_556 ?
O1 C1 1.252(2) . ?
O1 K1 2.7236(13) 1_455 ?
O1 K1 2.7445(12) 3_567 ?
C3 C2 1.398(2) . ?
C3 C1 1.402(2) . ?
C3 K1 3.2086(16) 2_556 ?
C3 H3 0.97(3) . ?
C1 C2 1.543(2) 3_466 ?
C1 K1 3.4538(15) 1_455 ?
C1 K1 3.5354(15) 3_567 ?
C2 C1 1.543(2) 3_466 ?
C2 K1 3.1674(14) 2_556 ?

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
O1 K1 O1 92.73(4) . 1_655 ?
O1 K1 O1 77.31(4) . 3_567 ?
O1 K1 O1 79.63(4) 1_655 3_567 ?
O1 K1 O2 93.48(4) . 2_446 ?
O1 K1 O2 171.80(4) 1_655 2_446 ?
O1 K1 O2 96.52(4) 3_567 2_446 ?
O1 K1 O2 58.39(4) . 3_466 ?
O1 K1 O2 85.81(4) 1_655 3_466 ?
O1 K1 O2 132.50(4) 3_567 3_466 ?
O2 K1 O2 102.01(4) 2_446 3_466 ?
O1 K1 O2 175.00(4) . 2_546 ?
O1 K1 O2 88.07(4) 1_655 2_546 ?
O1 K1 O2 98.00(4) 3_567 2_546 ?
O2 K1 O2 85.28(4) 2_446 2_546 ?
O2 K1 O2 126.61(3) 3_466 2_546 ?
O1 K1 C2 159.94(4) . 2_546 ?
O1 K1 C2 101.42(4) 1_655 2_546 ?
O1 K1 C2 118.95(4) 3_567 2_546 ?
O2 K1 C2 73.97(4) 2_446 2_546 ?
O2 K1 C2 108.15(4) 3_466 2_546 ?
O2 K1 C2 23.32(4) 2_546 2_546 ?
O1 K1 C3 140.50(4) . 2_546 ?
O1 K1 C3 94.42(4) 1_655 2_546 ?
O1 K1 C3 142.18(4) 3_567 2_546 ?
O2 K1 C3 84.16(4) 2_446 2_546 ?
O2 K1 C3 83.47(4) 3_466 2_546 ?
O2 K1 C3 44.24(4) 2_546 2_546 ?
C2 K1 C3 25.32(4) 2_546 2_546 ?
O1 K1 C1 81.46(4) . 1_655 ?
O1 K1 C1 19.08(4) 1_655 1_655 ?
O1 K1 C1 92.15(4) 3_567 1_655 ?
O2 K1 C1 168.78(4) 2_446 1_655 ?
O2 K1 C1 66.80(4) 3_466 1_655 ?
O2 K1 C1 100.59(4) 2_546 1_655 ?
C2 K1 C1 107.91(4) 2_546 1_655 ?
C3 K1 C1 93.36(4) 2_546 1_655 ?
O1 K1 C1 17.81(4) . . ?
O1 K1 C1 83.26(3) 1_655 . ?
O1 K1 C1 90.43(3) 3_567 . ?
O2 K1 C1 104.11(4) 2_446 . ?
O2 K1 C1 42.77(3) 3_466 . ?
O2 K1 C1 166.65(4) 2_546 . ?
C2 K1 C1 150.61(4) 2_546 . ?
C3 K1 C1 126.24(4) 2_546 . ?
C1 K1 C1 68.60(3) 1_655 . ?
O1 K1 C1 90.65(3) . 3_567 ?
O1 K1 C1 90.76(3) 1_655 3_567 ?
O1 K1 C1 17.92(4) 3_567 3_567 ?
O2 K1 C1 83.83(4) 2_446 3_567 ?
O2 K1 C1 148.55(4) 3_466 3_567 ?
O2 K1 C1 84.40(4) 2_546 3_567 ?
C2 K1 C1 103.17(4) 2_546 3_567 ?
C3 K1 C1 127.98(4) 2_546 3_567 ?
C1 K1 C1 106.14(3) 1_655 3_567 ?
C1 K1 C1 105.78(3) . 3_567 ?
O1 K1 K1 136.12(3) . 1_655 ?
O1 K1 K1 43.39(3) 1_655 1_655 ?
O1 K1 K1 91.50(3) 3_567 1_655 ?
O2 K1 K1 130.17(3) 2_446 1_655 ?
O2 K1 K1 108.05(3) 3_466 1_655 ?
O2 K1 K1 44.89(3) 2_546 1_655 ?
C2 K1 K1 59.43(3) 2_546 1_655 ?
C3 K1 K1 61.50(3) 2_546 1_655 ?
C1 K1 K1 56.39(3) 1_655 1_655 ?
C1 K1 K1 124.99(3) . 1_655 ?
C1 K1 K1 90.08(2) 3_567 1_655 ?
C2 O2 K1 119.89(11) . 2_456 ?
C2 O2 K1 116.64(10) . 3_466 ?
K1 O2 K1 110.34(4) 2_456 3_466 ?
C2 O2 K1 85.40(9) . 2_556 ?
K1 O2 K1 85.28(3) 2_456 2_556 ?
K1 O2 K1 136.48(5) 3_466 2_556 ?
C1 O1 K1 120.91(10) . . ?
C1 O1 K1 115.59(10) . 1_455 ?
K1 O1 K1 92.73(4) . 1_455 ?
C1 O1 K1 119.66(10) . 3_567 ?
K1 O1 K1 102.69(4) . 3_567 ?
K1 O1 K1 100.37(4) 1_455 3_567 ?
C2 C3 C1 122.62(14) . . ?
C2 C3 K1 75.69(9) . 2_556 ?
C1 C3 K1 123.12(10) . 2_556 ?
C2 C3 H3 117.7(16) . . ?
C1 C3 H3 119.6(16) . . ?
K1 C3 H3 73.6(15) 2_556 . ?
O1 C1 C3 123.80(15) . . ?
O1 C1 C2 117.25(14) . 3_466 ?
C3 C1 C2 118.94(14) . 3_466 ?
O1 C1 K1 45.34(8) . 1_455 ?
C3 C1 K1 115.65(10) . 1_455 ?
C2 C1 K1 105.49(9) 3_466 1_455 ?
O1 C1 K1 41.28(8) . . ?
C3 C1 K1 156.51(10) . . ?
C2 C1 K1 79.28(9) 3_466 . ?
K1 C1 K1 68.60(3) 1_455 . ?
O1 C1 K1 42.42(8) . 3_567 ?
C3 C1 K1 84.68(9) . 3_567 ?
C2 C1 K1 151.73(10) 3_466 3_567 ?
K1 C1 K1 73.86(3) 1_455 3_567 ?
K1 C1 K1 74.22(3) . 3_567 ?
O2 C2 C3 124.26(15) . . ?
O2 C2 C1 117.28(15) . 3_466 ?
C3 C2 C1 118.44(13) . 3_466 ?
O2 C2 K1 71.28(9) . 2_556 ?
C3 C2 K1 78.99(9) . 2_556 ?
C1 C2 K1 121.73(10) 3_466 2_556 ?

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
O1 K1 O1 C1 57.83(13) 1_655 . . . ?
O1 K1 O1 C1 136.56(14) 3_567 . . . ?
O2 K1 O1 C1 -127.53(12) 2_446 . . . ?
O2 K1 O1 C1 -25.56(11) 3_466 . . . ?
O2 K1 O1 C1 156.9(4) 2_546 . . . ?
C2 K1 O1 C1 -77.31(17) 2_546 . . . ?
C3 K1 O1 C1 -42.49(14) 2_546 . . . ?
C1 K1 O1 C1 42.39(10) 1_655 . . . ?
C1 K1 O1 C1 148.61(10) 3_567 . . . ?
K1 K1 O1 C1 57.83(13) 1_655 . . . ?
O1 K1 O1 K1 180 1_655 . . 1_455 ?
O1 K1 O1 K1 -101.27(4) 3_567 . . 1_455 ?
O2 K1 O1 K1 -5.36(4) 2_446 . . 1_455 ?
O2 K1 O1 K1 96.61(5) 3_466 . . 1_455 ?
O2 K1 O1 K1 -80.9(4) 2_546 . . 1_455 ?
C2 K1 O1 K1 44.86(13) 2_546 . . 1_455 ?
C3 K1 O1 K1 79.68(6) 2_546 . . 1_455 ?
C1 K1 O1 K1 164.57(4) 1_655 . . 1_455 ?
C1 K1 O1 K1 122.17(13) . . . 1_455 ?
C1 K1 O1 K1 -89.21(3) 3_567 . . 1_455 ?
K1 K1 O1 K1 180 1_655 . . 1_455 ?
O1 K1 O1 K1 -78.73(4) 1_655 . . 3_567 ?
O1 K1 O1 K1 0 3_567 . . 3_567 ?
O2 K1 O1 K1 95.91(4) 2_446 . . 3_567 ?
O2 K1 O1 K1 -162.12(6) 3_466 . . 3_567 ?
O2 K1 O1 K1 20.4(4) 2_546 . . 3_567 ?
C2 K1 O1 K1 146.13(11) 2_546 . . 3_567 ?
C3 K1 O1 K1 -179.05(5) 2_546 . . 3_567 ?
C1 K1 O1 K1 -94.17(4) 1_655 . . 3_567 ?
C1 K1 O1 K1 -136.56(14) . . . 3_567 ?
C1 K1 O1 K1 12.06(4) 3_567 . . 3_567 ?
K1 K1 O1 K1 -78.73(4) 1_655 . . 3_567 ?
K1 O1 C1 C3 -155.55(12) . . . . ?
K1 O1 C1 C3 94.06(15) 1_455 . . . ?
K1 O1 C1 C3 -26.1(2) 3_567 . . . ?
K1 O1 C1 C2 25.35(18) . . . 3_466 ?
K1 O1 C1 C2 -85.03(14) 1_455 . . 3_466 ?
K1 O1 C1 C2 154.82(10) 3_567 . . 3_466 ?
K1 O1 C1 K1 110.38(11) . . . 1_455 ?
K1 O1 C1 K1 -120.15(12) 3_567 . . 1_455 ?
K1 O1 C1 K1 -110.38(11) 1_455 . . . ?
K1 O1 C1 K1 129.47(14) 3_567 . . . ?
K1 O1 C1 K1 -129.47(14) . . . 3_567 ?
K1 O1 C1 K1 120.15(12) 1_455 . . 3_567 ?
C2 C3 C1 O1 -178.93(15) . . . . ?
K1 C3 C1 O1 87.23(18) 2_556 . . . ?
C2 C3 C1 C2 0.1(3) . . . 3_466 ?
K1 C3 C1 C2 -93.70(15) 2_556 . . 3_466 ?
C2 C3 C1 K1 -127.02(14) . . . 1_455 ?
K1 C3 C1 K1 139.14(7) 2_556 . . 1_455 ?
C2 C3 C1 K1 137.8(2) . . . . ?
K1 C3 C1 K1 44.0(3) 2_556 . . . ?
C2 C3 C1 K1 163.74(15) . . . 3_567 ?
K1 C3 C1 K1 69.89(9) 2_556 . . 3_567 ?
O1 K1 C1 O1 -121.64(13) 1_655 . . . ?
O1 K1 C1 O1 -42.13(13) 3_567 . . . ?
O2 K1 C1 O1 54.70(12) 2_446 . . . ?
O2 K1 C1 O1 147.25(14) 3_466 . . . ?
O2 K1 C1 O1 -171.50(13) 2_546 . . . ?
C2 K1 C1 O1 137.02(12) 2_546 . . . ?
C3 K1 C1 O1 147.81(11) 2_546 . . . ?
C1 K1 C1 O1 -134.27(11) 1_655 . . . ?
C1 K1 C1 O1 -32.76(11) 3_567 . . . ?
K1 K1 C1 O1 -134.27(11) 1_655 . . . ?
O1 K1 C1 C3 59.6(3) . . . . ?
O1 K1 C1 C3 -62.0(3) 1_655 . . . ?
O1 K1 C1 C3 17.5(3) 3_567 . . . ?
O2 K1 C1 C3 114.3(3) 2_446 . . . ?
O2 K1 C1 C3 -153.1(3) 3_466 . . . ?
O2 K1 C1 C3 -111.9(3) 2_546 . . . ?
C2 K1 C1 C3 -163.3(2) 2_546 . . . ?
C3 K1 C1 C3 -152.6(2) 2_546 . . . ?
C1 K1 C1 C3 -74.6(3) 1_655 . . . ?
C1 K1 C1 C3 26.9(3) 3_567 . . . ?
K1 K1 C1 C3 -74.6(3) 1_655 . . . ?
O1 K1 C1 C2 -157.20(17) . . . 3_466 ?
O1 K1 C1 C2 81.15(8) 1_655 . . 3_466 ?
O1 K1 C1 C2 160.66(8) 3_567 . . 3_466 ?
O2 K1 C1 C2 -102.50(9) 2_446 . . 3_466 ?
O2 K1 C1 C2 -9.96(8) 3_466 . . 3_466 ?
O2 K1 C1 C2 31.30(19) 2_546 . . 3_466 ?
C2 K1 C1 C2 -20.18(11) 2_546 . . 3_466 ?
C3 K1 C1 C2 -9.40(10) 2_546 . . 3_466 ?
C1 K1 C1 C2 68.53(8) 1_655 . . 3_466 ?
C1 K1 C1 C2 170.03(9) 3_567 . . 3_466 ?
K1 K1 C1 C2 68.53(8) 1_655 . . 3_466 ?
O1 K1 C1 K1 -45.73(11) . . . 1_455 ?
O1 K1 C1 K1 -167.37(3) 1_655 . . 1_455 ?
O1 K1 C1 K1 -87.86(3) 3_567 . . 1_455 ?
O2 K1 C1 K1 8.97(4) 2_446 . . 1_455 ?
O2 K1 C1 K1 101.51(5) 3_466 . . 1_455 ?
O2 K1 C1 K1 142.77(14) 2_546 . . 1_455 ?
C2 K1 C1 K1 91.29(8) 2_546 . . 1_455 ?
C3 K1 C1 K1 102.08(4) 2_546 . . 1_455 ?
C1 K1 C1 K1 180 1_655 . . 1_455 ?
C1 K1 C1 K1 -78.49(2) 3_567 . . 1_455 ?
K1 K1 C1 K1 180 1_655 . . 1_455 ?
O1 K1 C1 K1 32.76(11) . . . 3_567 ?
O1 K1 C1 K1 -88.88(3) 1_655 . . 3_567 ?
O1 K1 C1 K1 -9.37(3) 3_567 . . 3_567 ?
O2 K1 C1 K1 87.47(3) 2_446 . . 3_567 ?
O2 K1 C1 K1 -179.99(6) 3_466 . . 3_567 ?
O2 K1 C1 K1 -138.74(14) 2_546 . . 3_567 ?
C2 K1 C1 K1 169.78(7) 2_546 . . 3_567 ?
C3 K1 C1 K1 -179.43(4) 2_546 . . 3_567 ?
C1 K1 C1 K1 -101.51(2) 1_655 . . 3_567 ?
C1 K1 C1 K1 0 3_567 . . 3_567 ?
K1 K1 C1 K1 -101.51(2) 1_655 . . 3_567 ?
K1 O2 C2 C3 -20.2(2) 2_456 . . . ?
K1 O2 C2 C3 -157.69(13) 3_466 . . . ?
K1 O2 C2 C3 61.65(16) 2_556 . . . ?
K1 O2 C2 C1 161.38(10) 2_456 . . 3_466 ?
K1 O2 C2 C1 23.92(18) 3_466 . . 3_466 ?
K1 O2 C2 C1 -116.75(13) 2_556 . . 3_466 ?
K1 O2 C2 K1 -81.87(8) 2_456 . . 2_556 ?
K1 O2 C2 K1 140.67(9) 3_466 . . 2_556 ?
C1 C3 C2 O2 -178.53(16) . . . . ?
K1 C3 C2 O2 -58.12(15) 2_556 . . . ?
C1 C3 C2 C1 -0.1(3) . . . 3_466 ?
K1 C3 C2 C1 120.26(13) 2_556 . . 3_466 ?
C1 C3 C2 K1 -120.41(15) . . . 2_556 ?


data_li2dhq-3
_database_code_depnum_ccdc_archive 'CCDC 889127'
#TrackingRef 'LiDHQ-cifdoc.cif'


_audit_creation_date             2010-03-05T13:39:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_moiety         'C6 H6 Li2 O6'
_chemical_formula_sum            'C6 H6 Li2 O6'
_chemical_formula_weight         187.99

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

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

_cell_length_a                   15.9708(7)
_cell_length_b                   6.4417(2)
_cell_length_c                   7.9093(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.462(5)
_cell_angle_gamma                90
_cell_volume                     728.45(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1302
_cell_measurement_theta_min      6.1856
_cell_measurement_theta_max      75.8707

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             304
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82387
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54179
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_reflns_number            1618
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         6.19
_diffrn_reflns_theta_max         76.05
_diffrn_reflns_theta_full        76.05
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_reflns_number_total             818
_reflns_number_gt                758
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_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/[\s^2^(Fo^2^)+(0.0748P)^2^+0.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         818
_refine_ls_number_parameters     96
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1084
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.269

#------------------ 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'
Li Li 0.001 0 '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
C2B C 0.48352(13) 0 0.6634(2) 0.0196(4) Uani 1 d S . .
O2B O 0.47926(9) 0 0.81795(17) 0.0262(4) Uani 1 d S . .
O1B O 0.64860(9) 0 0.84493(17) 0.0240(3) Uani 1 d S . .
O5 O 0.81246(7) -0.24530(15) 0.80458(14) 0.0286(3) Uani 1 d D . .
C1B C 0.58289(12) 0 0.6789(2) 0.0187(4) Uani 1 d S . .
Li2 Li 0.7821(2) 0 0.9281(5) 0.0299(7) Uani 1 d S . .
Li1 Li 0.3974(2) 0 0.9486(4) 0.0270(7) Uani 1 d S . .
H3B H 0.3414(17) 0 0.473(4) 0.028(6) Uiso 1 d S . .
H3A H 0.0074(18) 0 0.816(4) 0.035(7) Uiso 1 d S . .
H5B H 0.8239(15) -0.191(4) 0.712(3) 0.056(6) Uiso 1 d D . .
H5A H 0.7580(16) -0.325(5) 0.739(4) 0.100(10) Uiso 1 d D . .
O1A O 0.16851(9) 0 0.80336(19) 0.0277(4) Uani 1 d S . .
O2A O 0.16012(10) 0 0.4631(2) 0.0300(4) Uani 1 d S . .
C2A C 0.08235(13) 0 0.4691(3) 0.0218(4) Uani 1 d S . .
C1A C 0.08736(13) 0 0.6678(2) 0.0209(4) Uani 1 d S . .
C3A C 0.00475(13) 0 0.6875(2) 0.0243(4) Uani 1 d S . .
C3B C 0.40600(12) 0 0.4862(2) 0.0207(4) Uani 1 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C2B 0.0220(9) 0.0215(8) 0.0172(8) 0 0.0105(7) 0
O2B 0.0239(7) 0.0413(8) 0.0156(6) 0 0.0107(5) 0
O1B 0.0197(7) 0.0354(7) 0.0143(6) 0 0.0053(5) 0
O5 0.0278(5) 0.0294(6) 0.0312(6) 0.0032(4) 0.0157(4) 0.0009(4)
C1B 0.0185(8) 0.0200(8) 0.0164(8) 0 0.0067(6) 0
Li2 0.0254(16) 0.0426(18) 0.0225(15) 0 0.0113(13) 0
Li1 0.0236(16) 0.0377(17) 0.0196(14) 0 0.0094(12) 0
O1A 0.0211(7) 0.0379(8) 0.0186(6) 0 0.0040(5) 0
O2A 0.0230(7) 0.0421(8) 0.0280(7) 0 0.0140(6) 0
C2A 0.0247(9) 0.0214(8) 0.0219(9) 0 0.0127(7) 0
C1A 0.0227(9) 0.0201(8) 0.0176(8) 0 0.0070(7) 0
C3A 0.0257(10) 0.0311(9) 0.0172(8) 0 0.0107(7) 0
C3B 0.0175(8) 0.0278(9) 0.0184(9) 0 0.0094(7) 0


#------------------ 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
C2B O2B 1.254(2) . ?
C2B C3B 1.397(2) . ?
C2B C1B 1.536(2) . ?
O2B Li1 1.996(3) . ?
O2B Li1 2.012(4) 5_657 ?
O1B C1B 1.264(2) . ?
O1B Li2 1.931(4) . ?
O1B Li1 2.068(3) 5_657 ?
O5 Li2 2.027(2) . ?
O5 Li1 2.110(2) 3_545 ?
O5 H5B 0.902(16) . ?
O5 H5A 0.942(18) . ?
C1B C3B 1.394(2) 5_656 ?
Li2 O1A 1.908(4) 5_657 ?
Li2 O5 2.027(2) 6 ?
Li2 Li1 3.415(5) 5_657 ?
Li1 O2B 2.012(4) 5_657 ?
Li1 O1B 2.068(3) 5_657 ?
Li1 O5 2.110(2) 8_445 ?
Li1 O5 2.110(2) 3_455 ?
Li1 Li1 3.005(6) 5_657 ?
Li1 Li2 3.415(5) 5_657 ?
O1A C1A 1.261(2) . ?
O1A Li2 1.908(4) 5_657 ?
O2A C2A 1.264(2) . ?
C2A C3A 1.391(3) 5_556 ?
C2A C1A 1.537(2) . ?
C1A C3A 1.396(3) . ?
C3A C2A 1.391(3) 5_556 ?
C3A H3A 0.99(3) . ?
C3B C1B 1.394(2) 5_656 ?
C3B H3B 0.99(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
O2B C2B C3B 124.71(16) . . ?
O2B C2B C1B 115.14(16) . . ?
C3B C2B C1B 120.15(16) . . ?
C2B O2B Li1 146.86(15) . . ?
C2B O2B Li1 115.99(15) . 5_657 ?
Li1 O2B Li1 97.15(13) . 5_657 ?
C1B O1B Li2 129.32(15) . . ?
C1B O1B Li1 113.45(15) . 5_657 ?
Li2 O1B Li1 117.24(15) . 5_657 ?
Li2 O5 Li1 125.46(12) . 3_545 ?
Li2 O5 H5B 105.8(16) . . ?
Li1 O5 H5B 115.1(15) 3_545 . ?
Li2 O5 H5A 109.3(19) . . ?
Li1 O5 H5A 95(2) 3_545 . ?
H5B O5 H5A 104(2) . . ?
O1B C1B C3B 125.44(16) . 5_656 ?
O1B C1B C2B 115.66(15) . . ?
C3B C1B C2B 118.90(16) 5_656 . ?
O1A Li2 O1B 103.02(17) 5_657 . ?
O1A Li2 O5 117.88(11) 5_657 . ?
O1B Li2 O5 107.49(12) . . ?
O1A Li2 O5 117.88(11) 5_657 6 ?
O1B Li2 O5 107.49(12) . 6 ?
O5 Li2 O5 102.44(16) . 6 ?
O1A Li2 Li1 70.45(12) 5_657 5_657 ?
O1B Li2 Li1 32.57(9) . 5_657 ?
O5 Li2 Li1 123.31(10) . 5_657 ?
O5 Li2 Li1 123.31(9) 6 5_657 ?
O2B Li1 O2B 82.85(13) . 5_657 ?
O2B Li1 O1B 162.62(18) . 5_657 ?
O2B Li1 O1B 79.77(13) 5_657 5_657 ?
O2B Li1 O5 97.60(11) . 8_445 ?
O2B Li1 O5 128.78(7) 5_657 8_445 ?
O1B Li1 O5 93.29(11) 5_657 8_445 ?
O2B Li1 O5 97.60(11) . 3_455 ?
O2B Li1 O5 128.78(7) 5_657 3_455 ?
O1B Li1 O5 93.29(11) 5_657 3_455 ?
O5 Li1 O5 102.08(14) 8_445 3_455 ?
O2B Li1 Li1 41.63(9) . 5_657 ?
O2B Li1 Li1 41.21(9) 5_657 5_657 ?
O1B Li1 Li1 120.98(19) 5_657 5_657 ?
O5 Li1 Li1 120.48(11) 8_445 5_657 ?
O5 Li1 Li1 120.48(11) 3_455 5_657 ?
O2B Li1 Li2 167.19(15) . 5_657 ?
O2B Li1 Li2 109.96(14) 5_657 5_657 ?
O1B Li1 Li2 30.19(8) 5_657 5_657 ?
O5 Li1 Li2 74.62(10) 8_445 5_657 ?
O5 Li1 Li2 74.62(10) 3_455 5_657 ?
Li1 Li1 Li2 151.17(18) 5_657 5_657 ?
C1A O1A Li2 134.81(16) . 5_657 ?
O2A C2A C3A 125.16(17) . 5_556 ?
O2A C2A C1A 115.73(16) . . ?
C3A C2A C1A 119.10(16) 5_556 . ?
O1A C1A C3A 124.71(17) . . ?
O1A C1A C2A 115.77(16) . . ?
C3A C1A C2A 119.52(16) . . ?
C2A C3A C1A 121.37(16) 5_556 . ?
C2A C3A H3A 118.6(15) 5_556 . ?
C1A C3A H3A 120.0(15) . . ?
C1B C3B C2B 120.94(15) 5_656 . ?
C1B C3B H3B 117.7(15) 5_656 . ?
C2B C3B H3B 121.3(15) . . ?

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
C3B C2B O2B Li1 0.0000(10) . . . . ?
C1B C2B O2B Li1 180.0000(10) . . . . ?
C3B C2B O2B Li1 180 . . . 5_657 ?
C1B C2B O2B Li1 0 . . . 5_657 ?
Li2 O1B C1B C3B 0 . . . 5_656 ?
Li1 O1B C1B C3B 180 5_657 . . 5_656 ?
Li2 O1B C1B C2B 180 . . . . ?
Li1 O1B C1B C2B 0 5_657 . . . ?
O2B C2B C1B O1B 0 . . . . ?
C3B C2B C1B O1B 180 . . . . ?
O2B C2B C1B C3B 180 . . . 5_656 ?
C3B C2B C1B C3B 0 . . . 5_656 ?
C1B O1B Li2 O1A 180 . . . 5_657 ?
Li1 O1B Li2 O1A 0 5_657 . . 5_657 ?
C1B O1B Li2 O5 -54.82(11) . . . . ?
Li1 O1B Li2 O5 125.18(11) 5_657 . . . ?
C1B O1B Li2 O5 54.82(11) . . . 6 ?
Li1 O1B Li2 O5 -125.18(11) 5_657 . . 6 ?
C1B O1B Li2 Li1 180.000(2) . . . 5_657 ?
Li1 O5 Li2 O1A -1.6(2) 3_545 . . 5_657 ?
Li1 O5 Li2 O1B -117.28(15) 3_545 . . . ?
Li1 O5 Li2 O5 129.62(13) 3_545 . . 6 ?
Li1 O5 Li2 Li1 -85.5(2) 3_545 . . 5_657 ?
C2B O2B Li1 O2B 180.0000(10) . . . 5_657 ?
Li1 O2B Li1 O2B 0 5_657 . . 5_657 ?
C2B O2B Li1 O1B 180.0000(10) . . . 5_657 ?
Li1 O2B Li1 O1B 0.000(2) 5_657 . . 5_657 ?
C2B O2B Li1 O5 51.67(8) . . . 8_445 ?
Li1 O2B Li1 O5 -128.33(8) 5_657 . . 8_445 ?
C2B O2B Li1 O5 -51.67(8) . . . 3_455 ?
Li1 O2B Li1 O5 128.33(8) 5_657 . . 3_455 ?
C2B O2B Li1 Li1 180.0000(10) . . . 5_657 ?
C2B O2B Li1 Li2 0.000(4) . . . 5_657 ?
Li1 O2B Li1 Li2 180.000(3) 5_657 . . 5_657 ?
Li2 O1A C1A C3A 0 5_657 . . . ?
Li2 O1A C1A C2A 180 5_657 . . . ?
O2A C2A C1A O1A 0 . . . . ?
C3A C2A C1A O1A 180 5_556 . . . ?
O2A C2A C1A C3A 180 . . . . ?
C3A C2A C1A C3A 0 5_556 . . . ?
O1A C1A C3A C2A 180 . . . 5_556 ?
C2A C1A C3A C2A 0 . . . 5_556 ?
O2B C2B C3B C1B 180 . . . 5_656 ?
C1B C2B C3B C1B 0 . . . 5_656 ?


data_nh4dhq-2
_database_code_depnum_ccdc_archive 'CCDC 889128'
#TrackingRef 'NH4DHQ-cifdoc.cif'


_audit_creation_date             2010-05-13T13:44:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_moiety         'C6 H2 O4, 2(H4 N)'
_chemical_formula_sum            'C6 H10 N2 O4 '
_chemical_formula_weight         174.16

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I b a m'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.2507(9)
_cell_length_b                   12.4085(13)
_cell_length_c                   7.0259(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     719.30(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    470
_cell_measurement_theta_min      6.4372
_cell_measurement_theta_max      75.241

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             368
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37382
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54179
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_reflns_number            772
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         6.44
_diffrn_reflns_theta_max         74.50
_diffrn_reflns_theta_full        75.41
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 0.939
_reflns_number_total             386
_reflns_number_gt                324
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_solution    'SIR97 (Giacovazzo et al, 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/[\s^2^(Fo^2^)+(0.1202P)^2^+0.8052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_number_reflns         386
_refine_ls_number_parameters     47
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1873
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.13
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.496

#------------------ 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'
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
H1A H 0.061(3) 0.3060(19) 0.172(4) 0.039(7) Uiso 1 d D . .
H3 H -0.154(4) 0.172(3) 0 0.036(10) Uiso 1 d S . .
H1B H 0.062(4) 0.374(3) 0.331(4) 0.063(10) Uiso 1 d D . .
O2 O 0.1607(2) 0.19016(15) 0 0.0352(8) Uani 1 d S . .
O1 O 0.3257(2) 0.00556(17) 0 0.0356(8) Uani 1 d S . .
C2 C 0.0783(3) 0.1036(2) 0 0.0273(8) Uani 1 d S . .
C3 C -0.0906(3) 0.0992(2) 0 0.0307(9) Uani 1 d S . .
C1 C 0.1743(3) -0.0018(2) 0 0.0244(8) Uani 1 d S . .
N1 N 0 0.3442(2) 0.25 0.0366(9) Uani 1 d SD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.0245(11) 0.0199(12) 0.0612(17) 0 0 -0.0043(7)
O1 0.0169(11) 0.0295(12) 0.0602(19) 0 0 0.0006(7)
C2 0.0226(15) 0.0197(13) 0.0396(18) 0 0 -0.0007(9)
C3 0.0212(15) 0.0188(13) 0.052(2) 0 0 0.0029(9)
C1 0.0197(13) 0.0242(14) 0.0292(19) 0 0 0.0021(9)
N1 0.0369(15) 0.0322(16) 0.0406(19) 0 0.0033(12) 0


#------------------ 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
O2 C2 1.270(3) . ?
O1 C1 1.252(3) . ?
C2 C3 1.395(4) . ?
C2 C1 1.530(4) . ?
C3 C1 1.392(4) 9 ?
C3 H3 1.04(4) . ?
C1 C3 1.392(4) 9 ?
N1 H1A 0.882(17) . ?
N1 H1B 0.849(18) . ?

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
O2 C2 C3 124.6(2) . . ?
O2 C2 C1 116.5(3) . . ?
C3 C2 C1 118.9(2) . . ?
C1 C3 C2 122.0(2) 9 . ?
C1 C3 H3 120(2) 9 . ?
C2 C3 H3 118(2) . . ?
O1 C1 C3 124.0(3) . 9 ?
O1 C1 C2 117.0(2) . . ?
C3 C1 C2 119.1(3) 9 . ?
H1A N1 H1B 108(3) . . ?

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
O2 C2 C3 C1 180 . . . 9 ?
C1 C2 C3 C1 0 . . . 9 ?
O2 C2 C1 O1 0 . . . . ?
C3 C2 C1 O1 180 . . . . ?
O2 C2 C1 C3 180 . . . 9 ?
C3 C2 C1 C3 0 . . . 9 ?


data_Rb2DHQ
_database_code_depnum_ccdc_archive 'CCDC 889129'
#TrackingRef 'RbDHQ-cifdoc.cif'


_audit_creation_date             2010-02-26T11:15:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_moiety         'C3 H1 O2 Rb'
_chemical_formula_sum            'C3 H1 O2 Rb'
_chemical_formula_weight         154.51

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I b a m'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.1716(4)
_cell_length_b                   12.4680(5)
_cell_length_c                   7.2307(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     736.69(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    407
_cell_measurement_theta_min      6.48
_cell_measurement_theta_max      75.48

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    17.029
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54179
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_number            850
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         6.48
_diffrn_reflns_theta_max         75.0
_diffrn_reflns_theta_full        75.48
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.969
_reflns_number_total             407
_reflns_number_gt                333
_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/[\s^2^(Fo^2^)+(0.0886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_number_reflns         407
_refine_ls_number_parameters     40
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1216
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_restrained_S_all      1.13
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.057

#------------------ 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'
Rb Rb -0.4688 1.6079 '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
H3 H -0.156(9) 0.177(5) 0 0.027(17) Uiso 1 d S . .
O2 O 0.1682(5) 0.1876(3) 0 0.0318(9) Uani 1 d S . .
O1 O 0.3303(6) -0.00051(15) 0 0.0263(11) Uani 1 d S . .
C2 C 0.0833(6) 0.1030(3) 0 0.0224(10) Uani 1 d S . .
C3 C -0.0857(6) 0.1002(3) 0 0.0245(10) Uani 1 d S . .
C1 C 0.1766(6) -0.0044(2) 0 0.0209(10) Uani 1 d S . .
Rb1 Rb 0 0.34613(3) 0.25 0.0304(5) Uani 1 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.0277(14) 0.0195(12) 0.0482(18) 0 0 -0.0081(15)
O1 0.0164(19) 0.026(2) 0.037(2) 0 0 0.0007(10)
C2 0.023(2) 0.019(2) 0.026(2) 0 0 -0.0038(15)
C3 0.022(2) 0.0169(19) 0.035(3) 0 0 0.0041(14)
C1 0.016(2) 0.024(2) 0.022(2) 0 0 0.0020(13)
Rb1 0.0380(6) 0.0262(6) 0.0270(6) 0 0.00279(14) 0


#------------------ 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
O2 C2 1.263(6) . ?
O2 Rb1 3.010(3) . ?
O2 Rb1 3.010(3) 10 ?
O2 Rb1 3.286(3) 13 ?
O2 Rb1 3.286(3) 6_554 ?
O1 C1 1.257(7) . ?
O1 Rb1 2.974(3) 5_544 ?
O1 Rb1 2.974(3) 14_545 ?
O1 Rb1 2.983(3) 13 ?
O1 Rb1 2.983(3) 6_554 ?
C2 C3 1.381(8) . ?
C2 C1 1.540(6) . ?
C2 Rb1 3.595(3) . ?
C2 Rb1 3.595(3) 10 ?
C3 C1 1.406(6) 9 ?
C3 Rb1 3.628(3) . ?
C3 Rb1 3.628(3) 10 ?
C3 H3 1.12(6) . ?
C1 C3 1.406(6) 9 ?
C1 Rb1 3.705(4) 14_545 ?
C1 Rb1 3.705(4) 5_544 ?
Rb1 O1 2.974(3) 15 ?
Rb1 O1 2.974(3) 5_455 ?
Rb1 O1 2.983(3) 13 ?
Rb1 O1 2.983(3) 7_454 ?
Rb1 O2 3.010(3) 11_556 ?
Rb1 O2 3.286(3) 13 ?
Rb1 O2 3.286(3) 7_454 ?
Rb1 C2 3.595(3) 11_556 ?
Rb1 Rb1 3.61535(14) 10_556 ?
Rb1 Rb1 3.61535(15) 10 ?
Rb1 H3 3.05(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O2 Rb1 107.3(2) . . ?
C2 O2 Rb1 107.3(2) . 10 ?
Rb1 O2 Rb1 73.81(9) . 10 ?
C2 O2 Rb1 110.3(2) . 13 ?
Rb1 O2 Rb1 97.49(5) . 13 ?
Rb1 O2 Rb1 142.29(13) 10 13 ?
C2 O2 Rb1 110.3(2) . 6_554 ?
Rb1 O2 Rb1 142.29(13) . 6_554 ?
Rb1 O2 Rb1 97.49(5) 10 6_554 ?
Rb1 O2 Rb1 66.75(8) 13 6_554 ?
C1 O1 Rb1 116.18(16) . 5_544 ?
C1 O1 Rb1 116.18(16) . 14_545 ?
Rb1 O1 Rb1 74.85(8) 5_544 14_545 ?
C1 O1 Rb1 119.30(16) . 13 ?
Rb1 O1 Rb1 124.50(17) 5_544 13 ?
Rb1 O1 Rb1 80.20(8) 14_545 13 ?
C1 O1 Rb1 119.30(16) . 6_554 ?
Rb1 O1 Rb1 80.20(8) 5_544 6_554 ?
Rb1 O1 Rb1 124.50(17) 14_545 6_554 ?
Rb1 O1 Rb1 74.61(8) 13 6_554 ?
O2 C2 C3 124.8(4) . . ?
O2 C2 C1 117.0(4) . . ?
C3 C2 C1 118.2(3) . . ?
O2 C2 Rb1 53.08(19) . . ?
C3 C2 Rb1 80.33(17) . . ?
C1 C2 Rb1 145.75(14) . . ?
O2 C2 Rb1 53.08(19) . 10 ?
C3 C2 Rb1 80.33(17) . 10 ?
C1 C2 Rb1 145.75(14) . 10 ?
Rb1 C2 Rb1 60.38(6) . 10 ?
C2 C3 C1 123.3(3) . 9 ?
C2 C3 Rb1 77.62(16) . . ?
C1 C3 Rb1 145.06(16) 9 . ?
C2 C3 Rb1 77.62(16) . 10 ?
C1 C3 Rb1 145.06(16) 9 10 ?
Rb1 C3 Rb1 59.77(6) . 10 ?
C2 C3 H3 119(3) . . ?
C1 C3 H3 117(3) 9 . ?
Rb1 C3 H3 51(3) . . ?
Rb1 C3 H3 51(3) 10 . ?
O1 C1 C3 124.1(3) . 9 ?
O1 C1 C2 117.5(3) . . ?
C3 C1 C2 118.5(4) 9 . ?
O1 C1 Rb1 46.09(12) . 14_545 ?
C3 C1 Rb1 87.1(2) 9 14_545 ?
C2 C1 Rb1 142.20(16) . 14_545 ?
O1 C1 Rb1 46.09(12) . 5_544 ?
C3 C1 Rb1 87.1(2) 9 5_544 ?
C2 C1 Rb1 142.20(16) . 5_544 ?
Rb1 C1 Rb1 58.41(6) 14_545 5_544 ?
O1 Rb1 O1 99.99(10) 15 5_455 ?
O1 Rb1 O1 74.73(7) 15 13 ?
O1 Rb1 O1 55.50(17) 5_455 13 ?
O1 Rb1 O1 55.50(17) 15 7_454 ?
O1 Rb1 O1 74.73(7) 5_455 7_454 ?
O1 Rb1 O1 99.62(9) 13 7_454 ?
O1 Rb1 O2 81.04(9) 15 . ?
O1 Rb1 O2 178.95(7) 5_455 . ?
O1 Rb1 O2 125.12(14) 13 . ?
O1 Rb1 O2 105.79(7) 7_454 . ?
O1 Rb1 O2 178.95(7) 15 11_556 ?
O1 Rb1 O2 81.04(9) 5_455 11_556 ?
O1 Rb1 O2 105.79(7) 13 11_556 ?
O1 Rb1 O2 125.12(14) 7_454 11_556 ?
O2 Rb1 O2 97.93(12) . 11_556 ?
O1 Rb1 O2 91.83(8) 15 13 ?
O1 Rb1 O2 97.63(8) 5_455 13 ?
O1 Rb1 O2 50.62(10) 13 13 ?
O1 Rb1 O2 143.10(11) 7_454 13 ?
O2 Rb1 O2 82.51(5) . 13 ?
O2 Rb1 O2 87.84(5) 11_556 13 ?
O1 Rb1 O2 97.63(8) 15 7_454 ?
O1 Rb1 O2 91.83(8) 5_455 7_454 ?
O1 Rb1 O2 143.10(11) 13 7_454 ?
O1 Rb1 O2 50.62(10) 7_454 7_454 ?
O2 Rb1 O2 87.84(5) . 7_454 ?
O2 Rb1 O2 82.51(5) 11_556 7_454 ?
O2 Rb1 O2 165.29(13) 13 7_454 ?
O1 Rb1 C2 98.53(6) 15 . ?
O1 Rb1 C2 159.40(10) 5_455 . ?
O1 Rb1 C2 139.55(11) 13 . ?
O1 Rb1 C2 109.12(5) 7_454 . ?
O2 Rb1 C2 19.59(10) . . ?
O2 Rb1 C2 80.49(7) 11_556 . ?
O2 Rb1 C2 90.71(9) 13 . ?
O2 Rb1 C2 76.80(9) 7_454 . ?
O1 Rb1 C2 159.40(10) 15 11_556 ?
O1 Rb1 C2 98.52(6) 5_455 11_556 ?
O1 Rb1 C2 109.12(5) 13 11_556 ?
O1 Rb1 C2 139.55(11) 7_454 11_556 ?
O2 Rb1 C2 80.49(7) . 11_556 ?
O2 Rb1 C2 19.59(10) 11_556 11_556 ?
O2 Rb1 C2 76.80(9) 13 11_556 ?
O2 Rb1 C2 90.71(9) 7_454 11_556 ?
C2 Rb1 C2 65.01(8) . 11_556 ?
O1 Rb1 Rb1 127.43(4) 15 10_556 ?
O1 Rb1 Rb1 52.57(4) 5_455 10_556 ?
O1 Rb1 Rb1 52.69(4) 13 10_556 ?
O1 Rb1 Rb1 127.31(4) 7_454 10_556 ?
O2 Rb1 Rb1 126.90(4) . 10_556 ?
O2 Rb1 Rb1 53.10(4) 11_556 10_556 ?
O2 Rb1 Rb1 56.62(4) 13 10_556 ?
O2 Rb1 Rb1 123.38(4) 7_454 10_556 ?
C2 Rb1 Rb1 120.19(3) . 10_556 ?
C2 Rb1 Rb1 59.81(3) 11_556 10_556 ?
O1 Rb1 Rb1 52.57(4) 15 10 ?
O1 Rb1 Rb1 127.43(4) 5_455 10 ?
O1 Rb1 Rb1 127.31(4) 13 10 ?
O1 Rb1 Rb1 52.69(4) 7_454 10 ?
O2 Rb1 Rb1 53.10(4) . 10 ?
O2 Rb1 Rb1 126.90(4) 11_556 10 ?
O2 Rb1 Rb1 123.38(4) 13 10 ?
O2 Rb1 Rb1 56.62(4) 7_454 10 ?
C2 Rb1 Rb1 59.81(3) . 10 ?
C2 Rb1 Rb1 120.19(3) 11_556 10 ?
Rb1 Rb1 Rb1 180 10_556 10 ?
O1 Rb1 H3 106.1(7) 15 . ?
O1 Rb1 H3 127.5(13) 5_455 . ?
O1 Rb1 H3 176.1(12) 13 . ?
O1 Rb1 H3 83.9(10) 7_454 . ?
O2 Rb1 H3 51.8(13) . . ?
O2 Rb1 H3 73.3(7) 11_556 . ?
O2 Rb1 H3 125.5(12) 13 . ?
O2 Rb1 H3 40.8(13) 7_454 . ?
C2 Rb1 H3 36.8(13) . . ?
C2 Rb1 H3 68.7(7) 11_556 . ?
Rb1 Rb1 H3 126.3(7) 10_556 . ?
Rb1 Rb1 H3 53.7(7) 10 . ?

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 O2 C2 C3 38.98(10) . . . . ?
Rb1 O2 C2 C3 -38.98(10) 10 . . . ?
Rb1 O2 C2 C3 144.09(10) 13 . . . ?
Rb1 O2 C2 C3 -144.09(10) 6_554 . . . ?
Rb1 O2 C2 C1 -141.02(10) . . . . ?
Rb1 O2 C2 C1 141.02(10) 10 . . . ?
Rb1 O2 C2 C1 -35.91(10) 13 . . . ?
Rb1 O2 C2 C1 35.91(10) 6_554 . . . ?
Rb1 O2 C2 Rb1 -77.95(19) 10 . . . ?
Rb1 O2 C2 Rb1 105.118(8) 13 . . . ?
Rb1 O2 C2 Rb1 176.93(19) 6_554 . . . ?
Rb1 O2 C2 Rb1 77.95(19) . . . 10 ?
Rb1 O2 C2 Rb1 -176.93(19) 13 . . 10 ?
Rb1 O2 C2 Rb1 -105.118(8) 6_554 . . 10 ?
O2 C2 C3 C1 180 . . . 9 ?
C1 C2 C3 C1 0 . . . 9 ?
Rb1 C2 C3 C1 -149.33(3) . . . 9 ?
Rb1 C2 C3 C1 149.33(3) 10 . . 9 ?
O2 C2 C3 Rb1 -30.67(3) . . . . ?
C1 C2 C3 Rb1 149.33(3) . . . . ?
Rb1 C2 C3 Rb1 -61.35(5) 10 . . . ?
O2 C2 C3 Rb1 30.67(3) . . . 10 ?
C1 C2 C3 Rb1 -149.33(3) . . . 10 ?
Rb1 C2 C3 Rb1 61.35(5) . . . 10 ?
Rb1 O1 C1 C3 42.63(8) 5_544 . . 9 ?
Rb1 O1 C1 C3 -42.63(8) 14_545 . . 9 ?
Rb1 O1 C1 C3 -135.97(9) 13 . . 9 ?
Rb1 O1 C1 C3 135.97(9) 6_554 . . 9 ?
Rb1 O1 C1 C2 -137.37(8) 5_544 . . . ?
Rb1 O1 C1 C2 137.37(8) 14_545 . . . ?
Rb1 O1 C1 C2 44.03(9) 13 . . . ?
Rb1 O1 C1 C2 -44.03(9) 6_554 . . . ?
Rb1 O1 C1 Rb1 85.25(16) 5_544 . . 14_545 ?
Rb1 O1 C1 Rb1 -93.346(16) 13 . . 14_545 ?
Rb1 O1 C1 Rb1 178.60(17) 6_554 . . 14_545 ?
Rb1 O1 C1 Rb1 -85.25(16) 14_545 . . 5_544 ?
Rb1 O1 C1 Rb1 -178.60(17) 13 . . 5_544 ?
Rb1 O1 C1 Rb1 93.346(16) 6_554 . . 5_544 ?
O2 C2 C1 O1 0 . . . . ?
C3 C2 C1 O1 180 . . . . ?
Rb1 C2 C1 O1 -63.3(4) . . . . ?
Rb1 C2 C1 O1 63.3(4) 10 . . . ?
O2 C2 C1 C3 180 . . . 9 ?
C3 C2 C1 C3 0 . . . 9 ?
Rb1 C2 C1 C3 116.7(4) . . . 9 ?
Rb1 C2 C1 C3 -116.7(4) 10 . . 9 ?
O2 C2 C1 Rb1 52.7(3) . . . 14_545 ?
C3 C2 C1 Rb1 -127.3(3) . . . 14_545 ?
Rb1 C2 C1 Rb1 -10.6(7) . . . 14_545 ?
Rb1 C2 C1 Rb1 116.07(16) 10 . . 14_545 ?
O2 C2 C1 Rb1 -52.7(3) . . . 5_544 ?
C3 C2 C1 Rb1 127.3(3) . . . 5_544 ?
Rb1 C2 C1 Rb1 -116.07(16) . . . 5_544 ?
Rb1 C2 C1 Rb1 10.6(7) 10 . . 5_544 ?
C2 O2 Rb1 O1 -152.93(19) . . . 15 ?
Rb1 O2 Rb1 O1 -49.38(11) 10 . . 15 ?
Rb1 O2 Rb1 O1 93.05(8) 13 . . 15 ?
Rb1 O2 Rb1 O1 31.78(17) 6_554 . . 15 ?
C2 O2 Rb1 O1 17(3) . . . 5_455 ?
Rb1 O2 Rb1 O1 120(3) 10 . . 5_455 ?
Rb1 O2 Rb1 O1 -97(3) 13 . . 5_455 ?
Rb1 O2 Rb1 O1 -159(3) 6_554 . . 5_455 ?
C2 O2 Rb1 O1 142.97(19) . . . 13 ?
Rb1 O2 Rb1 O1 -113.48(6) 10 . . 13 ?
Rb1 O2 Rb1 O1 28.95(10) 13 . . 13 ?
Rb1 O2 Rb1 O1 -32.31(15) 6_554 . . 13 ?
C2 O2 Rb1 O1 -102.8(2) . . . 7_454 ?
Rb1 O2 Rb1 O1 0.79(8) 10 . . 7_454 ?
Rb1 O2 Rb1 O1 143.23(11) 13 . . 7_454 ?
Rb1 O2 Rb1 O1 81.96(12) 6_554 . . 7_454 ?
C2 O2 Rb1 O2 27.27(17) . . . 11_556 ?
Rb1 O2 Rb1 O2 130.81(11) 10 . . 11_556 ?
Rb1 O2 Rb1 O2 -86.75(6) 13 . . 11_556 ?
Rb1 O2 Rb1 O2 -148.02(18) 6_554 . . 11_556 ?
C2 O2 Rb1 O2 114.0(2) . . . 13 ?
Rb1 O2 Rb1 O2 -142.43(12) 10 . . 13 ?
Rb1 O2 Rb1 O2 0 13 . . 13 ?
Rb1 O2 Rb1 O2 -61.27(14) 6_554 . . 13 ?
C2 O2 Rb1 O2 -54.86(17) . . . 7_454 ?
Rb1 O2 Rb1 O2 48.69(7) 10 . . 7_454 ?
Rb1 O2 Rb1 O2 -168.88(11) 13 . . 7_454 ?
Rb1 O2 Rb1 O2 129.85(18) 6_554 . . 7_454 ?
Rb1 O2 Rb1 C2 103.5(2) 10 . . . ?
Rb1 O2 Rb1 C2 -114.0(2) 13 . . . ?
Rb1 O2 Rb1 C2 -175.3(3) 6_554 . . . ?
C2 O2 Rb1 C2 36.2(2) . . . 11_556 ?
Rb1 O2 Rb1 C2 139.77(9) 10 . . 11_556 ?
Rb1 O2 Rb1 C2 -77.79(9) 13 . . 11_556 ?
Rb1 O2 Rb1 C2 -139.06(15) 6_554 . . 11_556 ?
C2 O2 Rb1 Rb1 76.5(2) . . . 10_556 ?
Rb1 O2 Rb1 Rb1 180 10 . . 10_556 ?
Rb1 O2 Rb1 Rb1 -37.57(12) 13 . . 10_556 ?
Rb1 O2 Rb1 Rb1 -98.83(12) 6_554 . . 10_556 ?
C2 O2 Rb1 Rb1 -103.5(2) . . . 10 ?
Rb1 O2 Rb1 Rb1 142.43(12) 13 . . 10 ?
Rb1 O2 Rb1 Rb1 81.17(12) 6_554 . . 10 ?
O2 C2 Rb1 O1 27.04(19) . . . 15 ?
C3 C2 Rb1 O1 -121.35(12) . . . 15 ?
C1 C2 Rb1 O1 111.7(4) . . . 15 ?
Rb1 C2 Rb1 O1 -37.04(10) 10 . . 15 ?
O2 C2 Rb1 O1 -179.14(14) . . . 5_455 ?
C3 C2 Rb1 O1 32.5(2) . . . 5_455 ?
C1 C2 Rb1 O1 -94.5(5) . . . 5_455 ?
Rb1 C2 Rb1 O1 116.78(17) 10 . . 5_455 ?
O2 C2 Rb1 O1 -49.4(2) . . . 13 ?
C3 C2 Rb1 O1 162.21(10) . . . 13 ?
C1 C2 Rb1 O1 35.2(5) . . . 13 ?
Rb1 C2 Rb1 O1 -113.47(6) 10 . . 13 ?
O2 C2 Rb1 O1 83.4(3) . . . 7_454 ?
C3 C2 Rb1 O1 -65.01(13) . . . 7_454 ?
C1 C2 Rb1 O1 168.0(4) . . . 7_454 ?
Rb1 C2 Rb1 O1 19.30(11) 10 . . 7_454 ?
C3 C2 Rb1 O2 -148.4(2) . . . . ?
C1 C2 Rb1 O2 84.6(5) . . . . ?
Rb1 C2 Rb1 O2 -64.08(18) 10 . . . ?
O2 C2 Rb1 O2 -152.61(17) . . . 11_556 ?
C3 C2 Rb1 O2 59.00(11) . . . 11_556 ?
C1 C2 Rb1 O2 -68.0(4) . . . 11_556 ?
Rb1 C2 Rb1 O2 143.31(8) 10 . . 11_556 ?
O2 C2 Rb1 O2 -64.92(19) . . . 13 ?
C3 C2 Rb1 O2 146.69(10) . . . 13 ?
C1 C2 Rb1 O2 19.7(5) . . . 13 ?
Rb1 C2 Rb1 O2 -129.00(6) 10 . . 13 ?
O2 C2 Rb1 O2 122.93(16) . . . 7_454 ?
C3 C2 Rb1 O2 -25.46(10) . . . 7_454 ?
C1 C2 Rb1 O2 -152.5(5) . . . 7_454 ?
Rb1 C2 Rb1 O2 58.85(6) 10 . . 7_454 ?
O2 C2 Rb1 C2 -140.0(3) . . . 11_556 ?
C3 C2 Rb1 C2 71.63(14) . . . 11_556 ?
C1 C2 Rb1 C2 -55.4(4) . . . 11_556 ?
Rb1 C2 Rb1 C2 155.94(15) 10 . . 11_556 ?
O2 C2 Rb1 Rb1 -115.92(18) . . . 10_556 ?
C3 C2 Rb1 Rb1 95.69(10) . . . 10_556 ?
C1 C2 Rb1 Rb1 -31.3(5) . . . 10_556 ?
Rb1 C2 Rb1 Rb1 180 10 . . 10_556 ?
O2 C2 Rb1 Rb1 64.08(18) . . . 10 ?
C3 C2 Rb1 Rb1 -84.31(10) . . . 10 ?
C1 C2 Rb1 Rb1 148.7(5) . . . 10 ?