# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_database_code_depnum_ccdc_archive 'CCDC 1528987'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C Li O3 Rb'
_chemical_formula_weight         152.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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                   6.849(3)
_cell_length_b                   7.162(3)
_cell_length_c                   7.525(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.961(5)
_cell_angle_gamma                90.00
_cell_volume                     334.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1053
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             280
_exptl_absorpt_coefficient_mu    14.597
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2566
_exptl_absorpt_correction_T_max  0.3599
_exptl_absorpt_process_details   face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1569
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         27.49
_reflns_number_total             765
_reflns_number_gt                670
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0289P)²+0.1084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         765
_refine_ls_number_parameters     55
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0512
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.16389(4) 0.35911(4) 0.33314(4) 0.01744(12) Uani 1 1 d . . .
O1 O 0.2971(3) 0.4721(3) 0.0261(3) 0.0158(4) Uani 1 1 d . . .
O2 O 0.1285(3) 0.1934(3) -0.0462(3) 0.0190(4) Uani 1 1 d . . .
O3 O 0.2264(4) 0.3336(3) -0.2586(3) 0.0196(5) Uani 1 1 d . . .
C C 0.2158(5) 0.3321(4) -0.0905(4) 0.0132(6) Uani 1 1 d . . .
Li1 Li 0.6033(8) 0.4284(8) 0.1956(7) 0.0176(10) Uani 1 1 d . . .


_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 O2 2.899(2) 2 ?
Rb1 O3 2.923(2) 1_556 ?
Rb1 O1 2.933(2) . ?
Rb1 O1 2.939(2) 2_545 ?
Rb1 O2 2.941(2) 4_666 ?
Rb1 O2 3.005(2) . ?
Rb1 O3 3.101(3) 4_566 ?
Rb1 C 3.313(3) 3_565 ?
Rb1 O3 3.322(2) 3_565 ?
Rb1 O1 3.396(2) 3_565 ?
Rb1 Li1 3.546(6) 2_545 ?
Rb1 Li1 3.558(5) 3_666 ?
O1 C 1.293(3) . ?
O1 Li1 1.966(5) . ?
O1 Li1 2.172(5) 3_665 ?
O1 Rb1 2.939(2) 2 ?
O1 Rb1 3.396(2) 3_565 ?
O2 C 1.274(3) . ?
O2 Li1 2.070(5) 4_565 ?
O2 Rb1 2.899(2) 2_545 ?
O2 Rb1 2.941(2) 4_565 ?
O3 C 1.297(3) . ?
O3 Li1 2.006(6) 3_665 ?
O3 Li1 2.026(6) 4_565 ?
O3 Rb1 2.923(2) 1_554 ?
O3 Rb1 3.101(3) 4_665 ?
O3 Rb1 3.322(2) 3_565 ?
C Li1 2.371(6) 4_565 ?
C Li1 2.435(6) 3_665 ?
C Rb1 3.313(3) 3_565 ?
C Rb1 3.621(3) 4_665 ?
Li1 O3 2.006(6) 3_665 ?
Li1 O3 2.026(6) 4_666 ?
Li1 O2 2.070(5) 4_666 ?
Li1 O1 2.172(5) 3_665 ?
Li1 C 2.371(6) 4_666 ?
Li1 C 2.435(6) 3_665 ?
Li1 Li1 2.865(10) 3_665 ?
Li1 Rb1 3.546(6) 2 ?
Li1 Rb1 3.558(5) 3_666 ?
Li1 Rb1 3.564(5) 1_655 ?
Li1 Rb1 3.579(5) 4_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
O2 Rb1 O3 69.54(6) 2 1_556 ?
O2 Rb1 O1 87.97(6) 2 . ?
O3 Rb1 O1 152.73(6) 1_556 . ?
O2 Rb1 O1 129.13(6) 2 2_545 ?
O3 Rb1 O1 67.15(6) 1_556 2_545 ?
O1 Rb1 O1 122.19(5) . 2_545 ?
O2 Rb1 O2 73.78(7) 2 4_666 ?
O3 Rb1 O2 90.46(6) 1_556 4_666 ?
O1 Rb1 O2 67.85(6) . 4_666 ?
O1 Rb1 O2 81.14(6) 2_545 4_666 ?
O2 Rb1 O2 132.51(5) 2 . ?
O3 Rb1 O2 152.98(6) 1_556 . ?
O1 Rb1 O2 44.60(6) . . ?
O1 Rb1 O2 85.89(6) 2_545 . ?
O2 Rb1 O2 83.45(5) 4_666 . ?
O2 Rb1 O3 133.89(6) 2 4_566 ?
O3 Rb1 O3 84.56(5) 1_556 4_566 ?
O1 Rb1 O3 122.68(6) . 4_566 ?
O1 Rb1 O3 65.98(6) 2_545 4_566 ?
O2 Rb1 O3 146.06(6) 4_666 4_566 ?
O2 Rb1 O3 85.97(5) . 4_566 ?
O2 Rb1 C 80.86(7) 2 3_565 ?
O3 Rb1 C 110.72(6) 1_556 3_565 ?
O1 Rb1 C 79.30(7) . 3_565 ?
O1 Rb1 C 139.38(7) 2_545 3_565 ?
O2 Rb1 C 138.64(6) 4_666 3_565 ?
O2 Rb1 C 90.58(7) . 3_565 ?
O3 Rb1 C 73.41(7) 4_566 3_565 ?
O2 Rb1 O3 73.62(6) 2 3_565 ?
O3 Rb1 O3 88.25(6) 1_556 3_565 ?
O1 Rb1 O3 100.35(6) . 3_565 ?
O1 Rb1 O3 129.06(6) 2_545 3_565 ?
O2 Rb1 O3 145.61(6) 4_666 3_565 ?
O2 Rb1 O3 111.38(6) . 3_565 ?
O3 Rb1 O3 67.93(3) 4_566 3_565 ?
C Rb1 O3 22.55(6) 3_565 3_565 ?
O2 Rb1 O1 102.73(6) 2 3_565 ?
O3 Rb1 O1 122.25(6) 1_556 3_565 ?
O1 Rb1 O1 76.61(6) . 3_565 ?
O1 Rb1 O1 122.36(6) 2_545 3_565 ?
O2 Rb1 O1 144.33(5) 4_666 3_565 ?
O2 Rb1 O1 73.09(6) . 3_565 ?
O3 Rb1 O1 59.66(6) 4_566 3_565 ?
C Rb1 O1 22.18(6) 3_565 3_565 ?
O3 Rb1 O1 38.59(5) 3_565 3_565 ?
O2 Rb1 Li1 150.74(9) 2 2_545 ?
O3 Rb1 Li1 81.52(9) 1_556 2_545 ?
O1 Rb1 Li1 121.06(9) . 2_545 ?
O1 Rb1 Li1 33.67(9) 2_545 2_545 ?
O2 Rb1 Li1 111.76(9) 4_666 2_545 ?
O2 Rb1 Li1 76.45(9) . 2_545 ?
O3 Rb1 Li1 34.31(9) 4_566 2_545 ?
C Rb1 Li1 106.39(10) 3_565 2_545 ?
O3 Rb1 Li1 102.02(9) 3_565 2_545 ?
O1 Rb1 Li1 88.78(9) 3_565 2_545 ?
O2 Rb1 Li1 35.57(9) 2 3_666 ?
O3 Rb1 Li1 34.32(9) 1_556 3_666 ?
O1 Rb1 Li1 120.63(9) . 3_666 ?
O1 Rb1 Li1 96.31(10) 2_545 3_666 ?
O2 Rb1 Li1 77.04(9) 4_666 3_666 ?
O2 Rb1 Li1 159.74(9) . 3_666 ?
O3 Rb1 Li1 113.37(9) 4_566 3_666 ?
C Rb1 Li1 100.44(10) 3_565 3_666 ?
O3 Rb1 Li1 82.83(9) 3_565 3_666 ?
O1 Rb1 Li1 121.07(9) 3_565 3_666 ?
Li1 Rb1 Li1 115.82(14) 2_545 3_666 ?
C O1 Li1 110.7(2) . . ?
C O1 Li1 85.3(2) . 3_665 ?
Li1 O1 Li1 87.5(2) . 3_665 ?
C O1 Rb1 97.62(16) . . ?
Li1 O1 Rb1 92.66(15) . . ?
Li1 O1 Rb1 176.83(17) 3_665 . ?
C O1 Rb1 157.40(18) . 2 ?
Li1 O1 Rb1 90.36(18) . 2 ?
Li1 O1 Rb1 87.53(16) 3_665 2 ?
Rb1 O1 Rb1 89.29(5) . 2 ?
C O1 Rb1 75.31(16) . 3_565 ?
Li1 O1 Rb1 162.13(17) . 3_565 ?
Li1 O1 Rb1 76.08(14) 3_665 3_565 ?
Rb1 O1 Rb1 103.39(6) . 3_565 ?
Rb1 O1 Rb1 82.16(5) 2 3_565 ?
C O2 Li1 86.9(2) . 4_565 ?
C O2 Rb1 127.87(18) . 2_545 ?
Li1 O2 Rb1 89.88(17) 4_565 2_545 ?
C O2 Rb1 125.79(19) . 4_565 ?
Li1 O2 Rb1 90.32(15) 4_565 4_565 ?
Rb1 O2 Rb1 106.22(7) 2_545 4_565 ?
C O2 Rb1 94.69(17) . . ?
Li1 O2 Rb1 178.31(19) 4_565 . ?
Rb1 O2 Rb1 88.67(6) 2_545 . ?
Rb1 O2 Rb1 89.25(5) 4_565 . ?
C O3 Li1 92.4(2) . 3_665 ?
C O3 Li1 88.2(2) . 4_565 ?
Li1 O3 Li1 170.3(2) 3_665 4_565 ?
C O3 Rb1 169.0(2) . 1_554 ?
Li1 O3 Rb1 90.44(15) 3_665 1_554 ?
Li1 O3 Rb1 90.77(15) 4_565 1_554 ?
C O3 Rb1 103.06(17) . 4_665 ?
Li1 O3 Rb1 85.11(17) 3_665 4_665 ?
Li1 O3 Rb1 85.37(15) 4_565 4_665 ?
Rb1 O3 Rb1 87.76(6) 1_554 4_665 ?
C O3 Rb1 78.33(16) . 3_565 ?
Li1 O3 Rb1 79.80(16) 3_665 3_565 ?
Li1 O3 Rb1 109.73(16) 4_565 3_565 ?
Rb1 O3 Rb1 91.75(6) 1_554 3_565 ?
Rb1 O3 Rb1 164.90(8) 4_665 3_565 ?
O2 C O1 122.8(3) . . ?
O2 C O3 119.1(3) . . ?
O1 C O3 118.1(3) . . ?
O2 C Li1 60.66(19) . 4_565 ?
O1 C Li1 173.9(2) . 4_565 ?
O3 C Li1 58.67(19) . 4_565 ?
O2 C Li1 173.4(2) . 3_665 ?
O1 C Li1 62.76(19) . 3_665 ?
O3 C Li1 55.40(19) . 3_665 ?
Li1 C Li1 113.44(13) 4_565 3_665 ?
O2 C Rb1 108.59(18) . 3_565 ?
O1 C Rb1 82.51(16) . 3_565 ?
O3 C Rb1 79.12(16) . 3_565 ?
Li1 C Rb1 101.34(16) 4_565 3_565 ?
Li1 C Rb1 74.89(14) 3_665 3_565 ?
O2 C Rb1 105.62(17) . 4_665 ?
O1 C Rb1 104.47(16) . 4_665 ?
O3 C Rb1 56.51(14) . 4_665 ?
Li1 C Rb1 69.43(13) 4_565 4_665 ?
Li1 C Rb1 68.49(14) 3_665 4_665 ?
Rb1 C Rb1 133.27(9) 3_565 4_665 ?
O1 Li1 O3 111.9(3) . 3_665 ?
O1 Li1 O3 120.7(3) . 4_666 ?
O3 Li1 O3 126.0(2) 3_665 4_666 ?
O1 Li1 O2 108.6(2) . 4_666 ?
O3 Li1 O2 109.1(3) 3_665 4_666 ?
O3 Li1 O2 65.54(18) 4_666 4_666 ?
O1 Li1 O1 92.5(2) . 3_665 ?
O3 Li1 O1 64.08(16) 3_665 3_665 ?
O3 Li1 O1 101.0(2) 4_666 3_665 ?
O2 Li1 O1 158.6(3) 4_666 3_665 ?
O1 Li1 C 121.2(3) . 4_666 ?
O3 Li1 C 121.2(2) 3_665 4_666 ?
O3 Li1 C 33.16(12) 4_666 4_666 ?
O2 Li1 C 32.46(12) 4_666 4_666 ?
O1 Li1 C 131.5(2) 3_665 4_666 ?
O1 Li1 C 103.1(2) . 3_665 ?
O3 Li1 C 32.16(12) 3_665 3_665 ?
O3 Li1 C 118.4(2) 4_666 3_665 ?
O2 Li1 C 138.6(3) 4_666 3_665 ?
O1 Li1 C 31.95(11) 3_665 3_665 ?
C Li1 C 135.3(2) 4_666 3_665 ?
O1 Li1 Li1 49.25(16) . 3_665 ?
O3 Li1 Li1 85.7(3) 3_665 3_665 ?
O3 Li1 Li1 119.7(3) 4_666 3_665 ?
O2 Li1 Li1 157.7(3) 4_666 3_665 ?
O1 Li1 Li1 43.29(14) 3_665 3_665 ?
C Li1 Li1 149.0(3) 4_666 3_665 ?
C Li1 Li1 60.82(19) 3_665 3_665 ?
O1 Li1 Rb1 55.97(15) . 2 ?
O3 Li1 Rb1 60.59(16) 3_665 2 ?
O3 Li1 Rb1 169.4(2) 4_666 2 ?
O2 Li1 Rb1 105.10(19) 4_666 2 ?
O1 Li1 Rb1 89.37(17) 3_665 2 ?
C Li1 Rb1 137.52(19) 4_666 2 ?
C Li1 Rb1 71.81(15) 3_665 2 ?
Li1 Li1 Rb1 66.9(2) 3_665 2 ?
O1 Li1 Rb1 119.0(2) . 3_666 ?
O3 Li1 Rb1 55.24(13) 3_665 3_666 ?
O3 Li1 Rb1 104.32(19) 4_666 3_666 ?
O2 Li1 Rb1 54.55(14) 4_666 3_666 ?
O1 Li1 Rb1 118.1(2) 3_665 3_666 ?
C Li1 Rb1 77.26(15) 4_666 3_666 ?
C Li1 Rb1 86.97(16) 3_665 3_666 ?
Li1 Li1 Rb1 133.7(3) 3_665 3_666 ?
Rb1 Li1 Rb1 72.03(10) 2 3_666 ?
O1 Li1 Rb1 159.1(2) . 1_655 ?
O3 Li1 Rb1 66.56(15) 3_665 1_655 ?
O3 Li1 Rb1 60.12(13) 4_666 1_655 ?
O2 Li1 Rb1 90.92(17) 4_666 1_655 ?
O1 Li1 Rb1 67.65(13) 3_665 1_655 ?
C Li1 Rb1 72.05(14) 4_666 1_655 ?
C Li1 Rb1 63.83(12) 3_665 1_655 ?
Li1 Li1 Rb1 110.7(2) 3_665 1_655 ?
Rb1 Li1 Rb1 127.14(15) 2 1_655 ?
Rb1 Li1 Rb1 78.20(10) 3_666 1_655 ?
O1 Li1 Rb1 91.84(18) . 4_665 ?
O3 Li1 Rb1 115.22(19) 3_665 4_665 ?
O3 Li1 Rb1 54.76(13) 4_666 4_665 ?
O2 Li1 Rb1 118.8(2) 4_666 4_665 ?
O1 Li1 Rb1 55.13(12) 3_665 4_665 ?
C Li1 Rb1 87.45(17) 4_666 4_665 ?
C Li1 Rb1 85.36(15) 3_665 4_665 ?
Li1 Li1 Rb1 65.70(19) 3_665 4_665 ?
Rb1 Li1 Rb1 132.59(15) 2 4_665 ?
Rb1 Li1 Rb1 149.13(15) 3_666 4_665 ?
Rb1 Li1 Rb1 71.58(9) 1_655 4_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.114
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_database_code_depnum_ccdc_archive 'CCDC 1528988'
_audit_update_record             
;
2017-01-22 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            LiCsCO3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C Cs Li O3'
_chemical_formula_weight         199.86

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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                   7.257(8)
_cell_length_b                   7.173(8)
_cell_length_c                   7.866(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.983(10)
_cell_angle_gamma                90.00
_cell_volume                     368.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    840
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             352
_exptl_absorpt_coefficient_mu    9.880
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3738
_exptl_absorpt_correction_T_max  0.4700
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2132
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.55
_reflns_number_total             840
_reflns_number_gt                789
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0249P)²+0.2310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0037(7)
_refine_ls_number_reflns         840
_refine_ls_number_parameters     55
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0438
_refine_ls_wR_factor_gt          0.0431
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.1021(8) 0.4247(8) 1.1857(7) 0.0207(10) Uani 1 1 d . . .
Cs1 Cs 0.16088(3) 0.13362(2) 0.82465(2) 0.02042(9) Uani 1 1 d . . .
C1 C -0.2208(5) -0.1676(4) 0.5999(4) 0.0151(5) Uani 1 1 d . . .
O1 O 0.1928(3) 0.5352(3) 0.9812(3) 0.0203(4) Uani 1 1 d . . .
O2 O 0.2350(4) 0.1652(3) 1.2424(3) 0.0226(5) Uani 1 1 d . . .
O3 O 0.3783(4) -0.2018(3) 1.0676(3) 0.0240(5) Uani 1 1 d . . .


_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
Li1 O1 1.981(6) 3_567 ?
Li1 O2 2.027(6) 2_557 ?
Li1 O2 2.054(6) . ?
Li1 O3 2.090(6) 2_557 ?
Li1 O1 2.139(6) . ?
Li1 C1 2.391(6) 3_557 ?
Li1 C1 2.430(6) 4_666 ?
Li1 C1 2.774(6) 2_456 ?
Li1 Li1 2.847(11) 3_567 ?
Li1 Cs1 3.681(6) 3_567 ?
Li1 Cs1 3.697(6) . ?
Li1 Cs1 3.732(7) 4_666 ?
Cs1 O3 3.048(3) . ?
Cs1 O2 3.097(4) . ?
Cs1 O1 3.102(4) . ?
Cs1 O1 3.107(3) 2_546 ?
Cs1 O3 3.108(4) 3_657 ?
Cs1 O3 3.198(4) 2_556 ?
Cs1 O2 3.209(4) 4_565 ?
Cs1 C1 3.343(4) . ?
Cs1 O2 3.435(4) 3_557 ?
Cs1 O1 3.502(3) 4_565 ?
Cs1 C1 3.560(5) 3_556 ?
Cs1 Li1 3.681(6) 3_567 ?
C1 O3 1.272(4) 4 ?
C1 O1 1.286(4) 4_565 ?
C1 O2 1.289(4) 3_557 ?
C1 Li1 2.391(6) 3_557 ?
C1 Li1 2.430(6) 4_565 ?
C1 Li1 2.774(6) 2_446 ?
C1 Cs1 3.560(5) 3_556 ?
C1 Cs1 3.774(4) 2_446 ?
C1 Cs1 3.869(4) 4 ?
O1 C1 1.286(4) 4_666 ?
O1 Li1 1.981(6) 3_567 ?
O1 Cs1 3.107(3) 2_556 ?
O1 Cs1 3.502(3) 4_666 ?
O2 C1 1.289(4) 3_557 ?
O2 Li1 2.027(6) 2_547 ?
O2 Cs1 3.209(4) 4_666 ?
O2 Cs1 3.435(4) 3_557 ?
O3 C1 1.272(4) 4_656 ?
O3 Li1 2.090(6) 2_547 ?
O3 Cs1 3.108(4) 3_657 ?
O3 Cs1 3.198(4) 2_546 ?
O3 Cs1 3.776(4) 4_656 ?

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 Li1 O2 113.0(3) 3_567 2_557 ?
O1 Li1 O2 122.9(3) 3_567 . ?
O2 Li1 O2 123.4(3) 2_557 . ?
O1 Li1 O3 107.1(3) 3_567 2_557 ?
O2 Li1 O3 108.4(3) 2_557 2_557 ?
O2 Li1 O3 64.55(19) . 2_557 ?
O1 Li1 O1 92.7(2) 3_567 . ?
O2 Li1 O1 63.92(18) 2_557 . ?
O2 Li1 O1 103.2(2) . . ?
O3 Li1 O1 160.2(3) 2_557 . ?
O1 Li1 C1 122.0(3) 3_567 3_557 ?
O2 Li1 C1 118.3(3) 2_557 3_557 ?
O2 Li1 C1 32.62(13) . 3_557 ?
O3 Li1 C1 32.11(12) 2_557 3_557 ?
O1 Li1 C1 133.0(3) . 3_557 ?
O1 Li1 C1 105.1(2) 3_567 4_666 ?
O2 Li1 C1 32.04(13) 2_557 4_666 ?
O2 Li1 C1 117.1(3) . 4_666 ?
O3 Li1 C1 137.7(3) 2_557 4_666 ?
O1 Li1 C1 31.88(12) . 4_666 ?
C1 Li1 C1 132.7(2) 3_557 4_666 ?
O1 Li1 C1 24.93(11) 3_567 2_456 ?
O2 Li1 C1 133.0(3) 2_557 2_456 ?
O2 Li1 C1 99.6(2) . 2_456 ?
O3 Li1 C1 106.7(2) 2_557 2_456 ?
O1 Li1 C1 90.3(2) . 2_456 ?
C1 Li1 C1 108.1(2) 3_557 2_456 ?
C1 Li1 C1 114.0(2) 4_666 2_456 ?
O1 Li1 Li1 48.64(17) 3_567 3_567 ?
O2 Li1 Li1 86.6(3) 2_557 3_567 ?
O2 Li1 Li1 123.4(3) . 3_567 ?
O3 Li1 Li1 155.6(4) 2_557 3_567 ?
O1 Li1 Li1 44.02(17) . 3_567 ?
C1 Li1 Li1 151.8(4) 3_557 3_567 ?
C1 Li1 Li1 62.8(2) 4_666 3_567 ?
C1 Li1 Li1 51.20(18) 2_456 3_567 ?
O1 Li1 Cs1 57.41(15) 3_567 3_567 ?
O2 Li1 Cs1 60.45(17) 2_557 3_567 ?
O2 Li1 Cs1 167.1(2) . 3_567 ?
O3 Li1 Cs1 102.6(2) 2_557 3_567 ?
O1 Li1 Cs1 89.52(18) . 3_567 ?
C1 Li1 Cs1 134.6(2) 3_557 3_567 ?
C1 Li1 Cs1 73.08(17) 4_666 3_567 ?
C1 Li1 Cs1 82.18(15) 2_456 3_567 ?
Li1 Li1 Cs1 67.6(2) 3_567 3_567 ?
O1 Li1 Cs1 91.6(2) 3_567 . ?
O2 Li1 Cs1 116.5(2) 2_557 . ?
O2 Li1 Cs1 56.88(15) . . ?
O3 Li1 Cs1 119.0(2) 2_557 . ?
O1 Li1 Cs1 56.95(15) . . ?
C1 Li1 Cs1 88.80(19) 3_557 . ?
C1 Li1 Cs1 86.46(18) 4_666 . ?
C1 Li1 Cs1 69.69(14) 2_456 . ?
Li1 Li1 Cs1 67.0(2) 3_567 . ?
Cs1 Li1 Cs1 134.61(15) 3_567 . ?
O1 Li1 Cs1 158.4(2) 3_567 4_666 ?
O2 Li1 Cs1 65.65(16) 2_557 4_666 ?
O2 Li1 Cs1 59.20(15) . 4_666 ?
O3 Li1 Cs1 93.21(18) 2_557 4_666 ?
O1 Li1 Cs1 66.99(15) . 4_666 ?
C1 Li1 Cs1 72.39(14) 3_557 4_666 ?
C1 Li1 Cs1 61.49(14) 4_666 4_666 ?
C1 Li1 Cs1 141.3(2) 2_456 4_666 ?
Li1 Li1 Cs1 110.7(3) 3_567 4_666 ?
Cs1 Li1 Cs1 126.10(15) 3_567 4_666 ?
Cs1 Li1 Cs1 71.66(10) . 4_666 ?
O3 Cs1 O2 65.83(7) . . ?
O3 Cs1 O1 123.79(9) . . ?
O2 Cs1 O1 64.06(6) . . ?
O3 Cs1 O1 92.73(8) . 2_546 ?
O2 Cs1 O1 151.51(7) . 2_546 ?
O1 Cs1 O1 121.82(6) . 2_546 ?
O3 Cs1 O3 75.74(8) . 3_657 ?
O2 Cs1 O3 91.90(6) . 3_657 ?
O1 Cs1 O3 82.04(6) . 3_657 ?
O1 Cs1 O3 63.57(7) 2_546 3_657 ?
O3 Cs1 O3 134.37(5) . 2_556 ?
O2 Cs1 O3 153.84(7) . 2_556 ?
O1 Cs1 O3 90.00(8) . 2_556 ?
O1 Cs1 O3 41.64(7) 2_546 2_556 ?
O3 Cs1 O3 80.51(5) 3_657 2_556 ?
O3 Cs1 O2 132.03(6) . 4_565 ?
O2 Cs1 O2 83.42(6) . 4_565 ?
O1 Cs1 O2 63.90(7) . 4_565 ?
O1 Cs1 O2 124.87(7) 2_546 4_565 ?
O3 Cs1 O2 144.13(8) 3_657 4_565 ?
O3 Cs1 O2 88.22(6) 2_556 4_565 ?
O3 Cs1 C1 84.42(10) . . ?
O2 Cs1 C1 109.09(7) . . ?
O1 Cs1 C1 135.29(8) . . ?
O1 Cs1 C1 85.91(9) 2_546 . ?
O3 Cs1 C1 142.11(7) 3_657 . ?
O3 Cs1 C1 91.46(9) 2_556 . ?
O2 Cs1 C1 71.49(10) 4_565 . ?
O3 Cs1 O2 76.82(9) . 3_557 ?
O2 Cs1 O2 87.33(6) . 3_557 ?
O1 Cs1 O2 123.53(7) . 3_557 ?
O1 Cs1 O2 106.62(7) 2_546 3_557 ?
O3 Cs1 O2 150.21(7) 3_657 3_557 ?
O3 Cs1 O2 111.56(6) 2_556 3_557 ?
O2 Cs1 O2 65.35(8) 4_565 3_557 ?
C1 Cs1 O2 21.88(7) . 3_557 ?
O3 Cs1 O1 105.75(8) . 4_565 ?
O2 Cs1 O1 120.18(8) . 4_565 ?
O1 Cs1 O1 120.39(7) . 4_565 ?
O1 Cs1 O1 82.49(10) 2_546 4_565 ?
O3 Cs1 O1 146.00(6) 3_657 4_565 ?
O3 Cs1 O1 74.77(8) 2_556 4_565 ?
O2 Cs1 O1 58.47(8) 4_565 4_565 ?
C1 Cs1 O1 21.49(6) . 4_565 ?
O2 Cs1 O1 37.09(6) 3_557 4_565 ?
O3 Cs1 C1 113.57(8) . 3_556 ?
O2 Cs1 C1 162.66(7) . 3_556 ?
O1 Cs1 C1 106.89(7) . 3_556 ?
O1 Cs1 C1 20.84(6) 2_546 3_556 ?
O3 Cs1 C1 71.69(7) 3_657 3_556 ?
O3 Cs1 C1 20.83(7) 2_556 3_556 ?
O2 Cs1 C1 106.42(7) 4_565 3_556 ?
C1 Cs1 C1 87.79(9) . 3_556 ?
O2 Cs1 C1 109.66(7) 3_557 3_556 ?
O1 Cs1 C1 77.05(9) 4_565 3_556 ?
O3 Cs1 Li1 144.51(10) . 3_567 ?
O2 Cs1 Li1 78.93(9) . 3_567 ?
O1 Cs1 Li1 32.55(10) . 3_567 ?
O1 Cs1 Li1 121.88(9) 2_546 3_567 ?
O3 Cs1 Li1 110.86(11) 3_657 3_567 ?
O3 Cs1 Li1 80.50(10) 2_556 3_567 ?
O2 Cs1 Li1 33.32(9) 4_565 3_567 ?
C1 Cs1 Li1 104.08(12) . 3_567 ?
O2 Cs1 Li1 98.22(12) 3_557 3_567 ?
O1 Cs1 Li1 87.84(11) 4_565 3_567 ?
C1 Cs1 Li1 101.28(10) 3_556 3_567 ?
O3 C1 O1 122.5(3) 4 4_565 ?
O3 C1 O2 119.5(3) 4 3_557 ?
O1 C1 O2 118.0(3) 4_565 3_557 ?
O3 C1 Li1 60.8(2) 4 3_557 ?
O1 C1 Li1 172.9(3) 4_565 3_557 ?
O2 C1 Li1 59.2(2) 3_557 3_557 ?
O3 C1 Li1 175.8(3) 4 4_565 ?
O1 C1 Li1 61.5(2) 4_565 4_565 ?
O2 C1 Li1 56.5(2) 3_557 4_565 ?
Li1 C1 Li1 115.35(15) 3_557 4_565 ?
O3 C1 Li1 117.7(2) 4 2_446 ?
O1 C1 Li1 40.50(18) 4_565 2_446 ?
O2 C1 Li1 107.7(2) 3_557 2_446 ?
Li1 C1 Li1 132.7(2) 3_557 2_446 ?
Li1 C1 Li1 66.0(2) 4_565 2_446 ?
O3 C1 Cs1 99.9(2) 4 . ?
O1 C1 Cs1 86.23(18) 4_565 . ?
O2 C1 Cs1 83.08(18) 3_557 . ?
Li1 C1 Cs1 99.58(17) 3_557 . ?
Li1 C1 Cs1 78.82(17) 4_565 . ?
Li1 C1 Cs1 125.14(16) 2_446 . ?
O3 C1 Cs1 63.35(16) 4 3_556 ?
O1 C1 Cs1 59.33(16) 4_565 3_556 ?
O2 C1 Cs1 174.8(2) 3_557 3_556 ?
Li1 C1 Cs1 124.07(17) 3_557 3_556 ?
Li1 C1 Cs1 120.57(17) 4_565 3_556 ?
Li1 C1 Cs1 73.29(15) 2_446 3_556 ?
Cs1 C1 Cs1 92.21(8) . 3_556 ?
O3 C1 Cs1 110.1(2) 4 2_446 ?
O1 C1 Cs1 102.47(19) 4_565 2_446 ?
O2 C1 Cs1 54.81(15) 3_557 2_446 ?
Li1 C1 Cs1 70.47(15) 3_557 2_446 ?
Li1 C1 Cs1 68.91(16) 4_565 2_446 ?
Li1 C1 Cs1 66.74(15) 2_446 2_446 ?
Cs1 C1 Cs1 136.31(10) . 2_446 ?
Cs1 C1 Cs1 129.27(8) 3_556 2_446 ?
O3 C1 Cs1 42.13(16) 4 4 ?
O1 C1 Cs1 108.3(2) 4_565 4 ?
O2 C1 Cs1 117.27(18) 3_557 4 ?
Li1 C1 Cs1 69.59(17) 3_557 4 ?
Li1 C1 Cs1 139.49(17) 4_565 4 ?
Li1 C1 Cs1 81.66(14) 2_446 4 ?
Cs1 C1 Cs1 141.60(10) . 4 ?
Cs1 C1 Cs1 67.83(7) 3_556 4 ?
Cs1 C1 Cs1 76.47(6) 2_446 4 ?
C1 O1 Li1 114.6(3) 4_666 3_567 ?
C1 O1 Li1 86.6(2) 4_666 . ?
Li1 O1 Li1 87.3(2) 3_567 . ?
C1 O1 Cs1 154.42(19) 4_666 . ?
Li1 O1 Cs1 90.03(18) 3_567 . ?
Li1 O1 Cs1 87.73(17) . . ?
C1 O1 Cs1 99.83(18) 4_666 2_556 ?
Li1 O1 Cs1 95.16(19) 3_567 2_556 ?
Li1 O1 Cs1 171.32(17) . 2_556 ?
Cs1 O1 Cs1 83.96(7) . 2_556 ?
C1 O1 Cs1 72.28(17) 4_666 4_666 ?
Li1 O1 Cs1 164.30(18) 3_567 4_666 ?
Li1 O1 Cs1 78.80(17) . 4_666 ?
Cs1 O1 Cs1 82.16(7) . 4_666 ?
Cs1 O1 Cs1 97.51(10) 2_556 4_666 ?
C1 O2 Li1 91.5(2) 3_557 2_547 ?
C1 O2 Li1 88.2(2) 3_557 . ?
Li1 O2 Li1 173.3(2) 2_547 . ?
C1 O2 Cs1 166.4(2) 3_557 . ?
Li1 O2 Cs1 92.46(17) 2_547 . ?
Li1 O2 Cs1 89.38(17) . . ?
C1 O2 Cs1 106.02(18) 3_557 4_666 ?
Li1 O2 Cs1 86.23(19) 2_547 4_666 ?
Li1 O2 Cs1 87.45(18) . 4_666 ?
Cs1 O2 Cs1 87.20(6) . 4_666 ?
C1 O2 Cs1 75.04(17) 3_557 3_557 ?
Li1 O2 Cs1 81.84(19) 2_547 3_557 ?
Li1 O2 Cs1 104.50(19) . 3_557 ?
Cs1 O2 Cs1 92.67(6) . 3_557 ?
Cs1 O2 Cs1 168.05(8) 4_666 3_557 ?
C1 O3 Li1 87.1(2) 4_656 2_547 ?
C1 O3 Cs1 121.6(2) 4_656 . ?
Li1 O3 Cs1 92.61(19) 2_547 . ?
C1 O3 Cs1 134.1(2) 4_656 3_657 ?
Li1 O3 Cs1 92.92(16) 2_547 3_657 ?
Cs1 O3 Cs1 104.26(8) . 3_657 ?
C1 O3 Cs1 95.82(18) 4_656 2_546 ?
Li1 O3 Cs1 175.82(19) 2_547 2_546 ?
Cs1 O3 Cs1 83.31(9) . 2_546 ?
Cs1 O3 Cs1 87.20(6) 3_657 2_546 ?
C1 O3 Cs1 60.72(18) 4_656 4_656 ?
Li1 O3 Cs1 93.38(18) 2_547 4_656 ?
Cs1 O3 Cs1 173.70(7) . 4_656 ?
Cs1 O3 Cs1 73.49(7) 3_657 4_656 ?
Cs1 O3 Cs1 90.66(8) 2_546 4_656 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.128

