# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_t
_database_code_depnum_ccdc_archive 'CCDC 1901350'
loop_
_audit_author_name
_audit_author_address
'Qi Wu'
;Hubei Normal University
China
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-16 downloaded from the CCDC.
;
_audit_creation_date             2019-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd2 I6, 2(H2 O), 2(Rb)'
_chemical_formula_sum            'Cd2 H4 I6 O2 Rb2'
_chemical_formula_weight         1193.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   8.7482(18)
_cell_length_b                   7.4018(15)
_cell_length_c                   14.741(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.113(4)
_cell_angle_gamma                90
_cell_volume                     954.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1313
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      20.66
_shelx_estimated_absorpt_T_max   0.484
_shelx_estimated_absorpt_T_min   0.282
_exptl_absorpt_coefficient_mu    16.974
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5335
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         2.752
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.498
_reflns_Friedel_fraction_full    0.500
_reflns_Friedel_fraction_max     0.500
_reflns_number_gt                1891
_reflns_number_total             2539
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.552
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.483
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2539
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0806
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1200P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.1975
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.2526(4) 0.3512(4) 0.2630(3) 0.0444(8) Uani 1 1 d . . . . .
Cd2 Cd 0.7527(3) 0.2978(4) 0.2401(2) 0.0424(8) Uani 1 1 d . . . . .
I1 I 0.5039(3) 0.4806(4) 0.1610(2) 0.0533(8) Uani 1 1 d . . . . .
I2 I 0.2597(4) -0.0166(4) 0.2670(3) 0.0571(9) Uani 1 1 d . . . . .
I3 I 0.0037(3) 0.4860(4) 0.1634(2) 0.0528(8) Uani 1 1 d . . . . .
I4 I 0.2576(5) 0.4936(5) 0.4303(3) 0.0621(9) Uani 1 1 d . . . . .
I5 I 0.7577(5) -0.0382(5) 0.1743(3) 0.0749(12) Uani 1 1 d . . . . .
I6 I 0.7597(4) 0.3151(4) 0.4239(2) 0.0543(8) Uani 1 1 d . . . . .
O1 O 1.091(4) 1.056(4) 0.526(2) 0.056(9) Uani 1 1 d . . . . .
H1A H 1.0610 1.0386 0.5802 0.085 Uiso 1 1 d R . . . .
H1B H 1.0630 1.1619 0.5109 0.085 Uiso 1 1 d R . . . .
O2 O 0.595(5) 0.797(4) 0.405(3) 0.071(10) Uani 1 1 d . . . . .
H2A H 0.5652 0.6900 0.4164 0.106 Uiso 1 1 d R . . . .
H2B H 0.5675 0.8195 0.3502 0.106 Uiso 1 1 d R . . . .
Rb1 Rb 0.9263(7) 0.7990(9) 0.4086(6) 0.098(2) Uani 1 1 d . . . . .
Rb2 Rb 0.4261(7) 0.9551(11) 0.0237(5) 0.094(2) 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
Cd1 I1 2.833(5) . ?
Cd1 I2 2.723(4) . ?
Cd1 I3 2.807(5) . ?
Cd1 I4 2.683(5) . ?
Cd2 I1 2.814(4) . ?
Cd2 I3 2.837(4) 1_655 ?
Cd2 I5 2.670(4) . ?
Cd2 I6 2.713(4) . ?
I1 Rb2 4.109(9) . ?
I2 Rb1 3.840(8) 1_445 ?
I2 Rb2 4.076(9) 2_565 ?
I2 Rb2 3.879(8) 1_545 ?
I3 Cd2 2.837(4) 1_455 ?
I4 Rb1 3.689(8) 1_455 ?
I4 Rb2 3.885(8) 2_565 ?
I5 Rb1 3.942(10) 1_545 ?
I5 Rb2 3.650(8) 1_545 ?
I6 Rb1 3.873(7) . ?
I6 Rb1 4.095(7) 1_545 ?
I6 Rb2 3.835(7) 2_565 ?
O1 H1A 0.8518 . ?
O1 H1B 0.8510 . ?
O1 Rb1 2.94(3) . ?
O1 Rb2 2.94(3) 2_675 ?
O2 H2A 0.8513 . ?
O2 H2B 0.8507 . ?
O2 Rb1 2.90(4) . ?
O2 Rb2 2.94(4) 2_575 ?
Rb1 I2 3.840(8) 1_665 ?
Rb1 I4 3.689(8) 1_655 ?
Rb1 I5 3.942(10) 1_565 ?
Rb1 I6 4.095(7) 1_565 ?
Rb1 H2A 3.2621 . ?
Rb1 H2B 3.2564 . ?
Rb1 Rb2 5.037(10) 2_575 ?
Rb1 Rb2 5.028(10) 2_675 ?
Rb2 I2 3.879(8) 1_565 ?
Rb2 I2 4.076(9) 2_564 ?
Rb2 I4 3.885(8) 2_564 ?
Rb2 I5 3.650(8) 1_565 ?
Rb2 I6 3.835(7) 2_564 ?
Rb2 O1 2.94(3) 2_474 ?
Rb2 O2 2.94(4) 2_574 ?
Rb2 Rb1 5.028(10) 2_474 ?
Rb2 Rb1 5.037(10) 2_574 ?

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
I2 Cd1 I1 109.40(14) . . ?
I2 Cd1 I3 112.60(16) . . ?
I3 Cd1 I1 101.79(14) . . ?
I4 Cd1 I1 110.11(17) . . ?
I4 Cd1 I2 111.85(17) . . ?
I4 Cd1 I3 110.62(16) . . ?
I1 Cd2 I3 101.40(12) . 1_655 ?
I5 Cd2 I1 108.10(16) . . ?
I5 Cd2 I3 107.42(16) . 1_655 ?
I5 Cd2 I6 113.99(16) . . ?
I6 Cd2 I1 114.01(14) . . ?
I6 Cd2 I3 111.01(14) . 1_655 ?
Cd1 I1 Rb2 114.99(14) . . ?
Cd2 I1 Cd1 102.59(13) . . ?
Cd2 I1 Rb2 137.92(15) . . ?
Cd1 I2 Rb1 110.50(16) . 1_445 ?
Cd1 I2 Rb2 92.42(17) . 1_545 ?
Cd1 I2 Rb2 85.24(17) . 2_565 ?
Rb1 I2 Rb2 140.34(19) 1_445 1_545 ?
Rb1 I2 Rb2 78.79(17) 1_445 2_565 ?
Rb2 I2 Rb2 136.9(2) 1_545 2_565 ?
Cd1 I3 Cd2 102.56(13) . 1_455 ?
Cd1 I4 Rb1 98.6(2) . 1_455 ?
Cd1 I4 Rb2 89.73(17) . 2_565 ?
Rb1 I4 Rb2 148.43(19) 1_455 2_565 ?
Cd2 I5 Rb1 88.44(17) . 1_545 ?
Cd2 I5 Rb2 102.71(18) . 1_545 ?
Rb2 I5 Rb1 145.51(19) 1_545 1_545 ?
Cd2 I6 Rb1 89.62(17) . . ?
Cd2 I6 Rb1 84.73(16) . 1_545 ?
Cd2 I6 Rb2 110.05(17) . 2_565 ?
Rb1 I6 Rb1 136.51(18) . 1_545 ?
Rb2 I6 Rb1 142.32(17) 2_565 . ?
Rb2 I6 Rb1 78.79(15) 2_565 1_545 ?
H1A O1 H1B 107.2 . . ?
Rb1 O1 H1A 107.9 . . ?
Rb1 O1 H1B 107.8 . . ?
Rb2 O1 H1A 108.1 2_675 . ?
Rb2 O1 H1B 107.8 2_675 . ?
Rb2 O1 Rb1 117.6(11) 2_675 . ?
H2A O2 H2B 107.0 . . ?
Rb1 O2 H2A 107.6 . . ?
Rb1 O2 H2B 107.2 . . ?
Rb1 O2 Rb2 119.2(13) . 2_575 ?
Rb2 O2 H2A 107.8 2_575 . ?
Rb2 O2 H2B 107.5 2_575 . ?
I2 Rb1 I5 72.44(17) 1_665 1_565 ?
I2 Rb1 I6 130.3(2) 1_665 . ?
I2 Rb1 I6 88.22(14) 1_665 1_565 ?
I2 Rb1 H2A 147.5 1_665 . ?
I2 Rb1 H2B 124.9 1_665 . ?
I2 Rb1 Rb2 52.69(13) 1_665 2_675 ?
I2 Rb1 Rb2 135.7(2) 1_665 2_575 ?
I4 Rb1 I2 70.58(14) 1_655 1_665 ?
I4 Rb1 I5 123.8(2) 1_655 1_565 ?
I4 Rb1 I6 73.98(14) 1_655 . ?
I4 Rb1 I6 147.82(19) 1_655 1_565 ?
I4 Rb1 H2A 127.3 1_655 . ?
I4 Rb1 H2B 143.9 1_655 . ?
I4 Rb1 Rb2 60.66(14) 1_655 2_675 ?
I4 Rb1 Rb2 151.1(2) 1_655 2_575 ?
I5 Rb1 I6 68.31(13) 1_565 1_565 ?
I5 Rb1 H2A 75.3 1_565 . ?
I5 Rb1 H2B 52.8 1_565 . ?
I5 Rb1 Rb2 82.01(16) 1_565 2_575 ?
I5 Rb1 Rb2 120.57(19) 1_565 2_675 ?
I6 Rb1 I5 101.17(19) . 1_565 ?
I6 Rb1 I6 136.51(18) . 1_565 ?
I6 Rb1 H2A 53.5 . . ?
I6 Rb1 H2A 83.3 1_565 . ?
I6 Rb1 H2B 72.3 . . ?
I6 Rb1 H2B 68.2 1_565 . ?
I6 Rb1 Rb2 87.30(16) 1_565 2_675 ?
I6 Rb1 Rb2 48.31(12) 1_565 2_575 ?
I6 Rb1 Rb2 89.27(15) . 2_575 ?
I6 Rb1 Rb2 130.0(2) . 2_675 ?
O1 Rb1 I2 73.7(7) . 1_665 ?
O1 Rb1 I4 87.8(6) . 1_655 ?
O1 Rb1 I5 119.9(7) . 1_565 ?
O1 Rb1 I6 138.3(7) . . ?
O1 Rb1 I6 62.5(6) . 1_565 ?
O1 Rb1 H2A 127.6 . . ?
O1 Rb1 H2B 126.5 . . ?
O1 Rb1 Rb2 31.2(6) . 2_675 ?
O1 Rb1 Rb2 89.6(6) . 2_575 ?
O2 Rb1 I2 138.7(8) . 1_665 ?
O2 Rb1 I4 141.6(6) . 1_655 ?
O2 Rb1 I5 67.1(8) . 1_565 ?
O2 Rb1 I6 69.5(6) . 1_565 ?
O2 Rb1 I6 67.7(6) . . ?
O2 Rb1 O1 120.2(10) . . ?
O2 Rb1 H2A 14.4 . . ?
O2 Rb1 H2B 14.5 . . ?
O2 Rb1 Rb2 151.3(8) . 2_675 ?
O2 Rb1 Rb2 30.6(7) . 2_575 ?
H2A Rb1 H2B 24.2 . . ?
Rb2 Rb1 H2A 40.1 2_575 . ?
Rb2 Rb1 H2A 156.8 2_675 . ?
Rb2 Rb1 H2B 155.4 2_675 . ?
Rb2 Rb1 H2B 40.1 2_575 . ?
Rb2 Rb1 Rb2 120.7(2) 2_675 2_575 ?
I1 Rb2 Rb1 109.36(17) . 2_574 ?
I1 Rb2 Rb1 128.22(19) . 2_474 ?
I2 Rb2 I1 127.7(2) 2_564 . ?
I2 Rb2 I1 69.70(15) 1_565 . ?
I2 Rb2 I2 135.9(2) 1_565 2_564 ?
I2 Rb2 I4 103.37(19) 1_565 2_564 ?
I2 Rb2 Rb1 87.47(18) 2_564 2_574 ?
I2 Rb2 Rb1 48.52(14) 2_564 2_474 ?
I2 Rb2 Rb1 128.3(2) 1_565 2_574 ?
I2 Rb2 Rb1 87.98(16) 1_565 2_474 ?
I4 Rb2 I1 60.41(14) 2_564 . ?
I4 Rb2 I2 68.40(14) 2_564 2_564 ?
I4 Rb2 Rb1 82.01(16) 2_564 2_474 ?
I4 Rb2 Rb1 121.25(19) 2_564 2_574 ?
I5 Rb2 I1 65.26(15) 1_565 . ?
I5 Rb2 I2 147.7(2) 1_565 2_564 ?
I5 Rb2 I2 74.71(17) 1_565 1_565 ?
I5 Rb2 I4 121.9(2) 1_565 2_564 ?
I5 Rb2 I6 68.63(14) 1_565 2_564 ?
I5 Rb2 Rb1 60.64(15) 1_565 2_574 ?
I5 Rb2 Rb1 152.9(2) 1_565 2_474 ?
I6 Rb2 I1 67.52(13) 2_564 . ?
I6 Rb2 I2 88.44(17) 2_564 2_564 ?
I6 Rb2 I2 132.1(2) 2_564 1_565 ?
I6 Rb2 I4 72.93(15) 2_564 2_564 ?
I6 Rb2 Rb1 136.2(2) 2_564 2_474 ?
I6 Rb2 Rb1 52.90(12) 2_564 2_574 ?
O1 Rb2 I1 97.8(6) 2_474 . ?
O1 Rb2 I2 67.3(7) 2_474 1_565 ?
O1 Rb2 I2 70.0(7) 2_474 2_564 ?
O1 Rb2 I4 66.5(6) 2_474 2_564 ?
O1 Rb2 I5 141.9(8) 2_474 1_565 ?
O1 Rb2 I6 138.7(7) 2_474 2_564 ?
O1 Rb2 O2 121.8(11) 2_474 2_574 ?
O1 Rb2 Rb1 152.0(7) 2_474 2_574 ?
O1 Rb2 Rb1 31.3(6) 2_474 2_474 ?
O2 Rb2 I1 138.2(8) 2_574 . ?
O2 Rb2 I2 63.5(8) 2_574 2_564 ?
O2 Rb2 I2 135.1(7) 2_574 1_565 ?
O2 Rb2 I4 120.8(8) 2_574 2_564 ?
O2 Rb2 I5 87.5(9) 2_574 1_565 ?
O2 Rb2 I6 73.3(7) 2_574 2_564 ?
O2 Rb2 Rb1 30.2(8) 2_574 2_574 ?
O2 Rb2 Rb1 90.5(8) 2_574 2_474 ?
Rb1 Rb2 Rb1 120.7(2) 2_474 2_574 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_130423b_0m
_database_code_depnum_ccdc_archive 'CCDC 1901351'
loop_
_audit_author_name
_audit_author_address
'Qi Wu'
;Hubei Normal University
China
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-16 downloaded from the CCDC.
;
_audit_creation_date             2019-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd2 I6, 2(H2 O), 2(Cs)'
_chemical_formula_sum            'Cd2 H4 Cs2 I6 O2'
_chemical_formula_weight         1288.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   8.9666(7)
_cell_length_b                   7.5492(6)
_cell_length_c                   14.9311(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.4280(10)
_cell_angle_gamma                90
_cell_volume                     1010.67(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4333
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      31.16
_cell_measurement_theta_min      2.70
_shelx_estimated_absorpt_T_max   0.319
_shelx_estimated_absorpt_T_min   0.319
_exptl_absorpt_coefficient_mu    14.796
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    4.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6628
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.698
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                3160
_reflns_number_total             3259
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.0034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0280P)²+1.9175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0669
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 O2(H2A,H2B), O1(H1A,H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.5783(14) -1.2831(18) -0.2677(11) 0.085(4) Uani 1 1 d . . . . .
H2A H -0.5458 -1.1623 -0.2572 0.102 Uiso 1 1 calc R . . . .
H2B H -0.5532 -1.3141 -0.3288 0.102 Uiso 1 1 calc R . . . .
I5 I -0.74550(11) -0.81753(12) -0.23332(6) 0.0505(2) Uani 1 1 d . . . . .
Cd2 Cd -0.74062(10) -0.80474(13) -0.41539(6) 0.0402(2) Uani 1 1 d . . . . .
Cd1 Cd -0.24050(11) -0.85682(13) -0.39308(7) 0.0421(2) Uani 1 1 d . . . . .
I1 I -0.49221(10) -0.97990(12) -0.49251(6) 0.0479(2) Uani 1 1 d . . . . .
I6 I -0.99117(10) -0.98986(12) -0.48743(6) 0.0484(2) Uani 1 1 d . . . . .
I2 I -0.24849(13) -0.99859(13) -0.22584(7) 0.0536(2) Uani 1 1 d . . . . .
I4 I -0.74882(13) -0.47235(13) -0.48401(8) 0.0602(3) Uani 1 1 d . . . . .
I3 I -0.24387(12) -0.49475(12) -0.39046(7) 0.0538(2) Uani 1 1 d . . . . .
Cs1 Cs -0.90954(12) -1.30564(15) -0.24456(10) 0.0727(3) Uani 1 1 d . . . . .
Cs2 Cs -0.41125(12) -0.53556(19) -0.13643(8) 0.0723(3) Uani 1 1 d . . . . .
O1 O -0.0770(14) -0.5762(17) -0.1274(9) 0.070(3) Uani 1 1 d . . . . .
H1A H -0.0508 -0.6949 -0.1465 0.084 Uiso 1 1 calc R . . . .
H1B H -0.0444 -0.5627 -0.0657 0.084 Uiso 1 1 calc R . . . .


_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 H2A 0.9700 . ?
O2 H2B 0.9700 . ?
O2 Cs1 2.998(13) . ?
O2 Cs2 3.110(15) 1_545 ?
I5 Cd2 2.7210(12) . ?
I5 Cs1 4.1378(14) 1_565 ?
I5 Cs1 3.9706(14) . ?
I5 Cs2 3.9423(15) . ?
Cd2 I1 2.8415(14) . ?
Cd2 I6 2.8497(13) . ?
Cd2 I4 2.7112(14) . ?
Cd1 I1 2.8481(13) . ?
Cd1 I6 2.8351(14) 1_655 ?
Cd1 I2 2.7182(14) . ?
Cd1 I3 2.7338(13) . ?
I1 Cs2 4.3067(17) 2_534 ?
I6 Cd1 2.8352(14) 1_455 ?
I6 Cs1 4.3965(17) . ?
I2 Cs1 3.8342(16) 1_655 ?
I2 Cs2 4.0199(17) . ?
I4 Cs1 4.4650(19) 2_534 ?
I4 Cs1 4.0645(19) 1_565 ?
I4 Cs2 3.8010(16) 2_544 ?
I3 Cs1 3.9590(15) 1_665 ?
I3 Cs2 4.1011(16) . ?
I3 Cs2 3.9636(15) 2_544 ?
Cs1 I5 4.1379(14) 1_545 ?
Cs1 I2 3.8341(16) 1_455 ?
Cs1 I4 4.0645(19) 1_545 ?
Cs1 I4 4.4650(19) 2_535 ?
Cs1 I3 3.9589(15) 1_445 ?
Cs1 Cs2 5.0956(18) 1_445 ?
Cs1 Cs2 5.0472(17) 1_545 ?
Cs1 O1 3.087(13) 1_445 ?
Cs2 O2 3.110(15) 1_565 ?
Cs2 I1 4.3067(17) 2_535 ?
Cs2 I4 3.8010(16) 2_545 ?
Cs2 I3 3.9637(15) 2_545 ?
Cs2 Cs1 5.0956(18) 1_665 ?
Cs2 Cs1 5.0472(17) 1_565 ?
Cs2 O1 3.014(12) . ?
O1 Cs1 3.087(13) 1_665 ?
O1 H1A 0.9700 . ?
O1 H1B 0.9700 . ?

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
H2A O2 H2B 108.0 . . ?
Cs1 O2 H2A 109.3 . . ?
Cs1 O2 H2B 109.3 . . ?
Cs1 O2 Cs2 111.4(5) . 1_545 ?
Cs2 O2 H2A 109.3 1_545 . ?
Cs2 O2 H2B 109.3 1_545 . ?
Cd2 I5 Cs1 86.26(4) . 1_565 ?
Cd2 I5 Cs1 89.97(4) . . ?
Cd2 I5 Cs2 109.24(4) . . ?
Cs1 I5 Cs1 137.18(4) . 1_565 ?
Cs2 I5 Cs1 142.84(3) . . ?
Cs2 I5 Cs1 77.27(3) . 1_565 ?
I5 Cd2 I1 114.01(4) . . ?
I5 Cd2 I6 109.95(4) . . ?
I1 Cd2 I6 103.71(4) . . ?
I4 Cd2 I5 114.19(5) . . ?
I4 Cd2 I1 107.26(5) . . ?
I4 Cd2 I6 106.99(5) . . ?
I6 Cd1 I1 104.49(4) 1_655 . ?
I2 Cd1 I1 108.92(5) . . ?
I2 Cd1 I6 110.08(5) . 1_655 ?
I2 Cd1 I3 112.34(5) . . ?
I3 Cd1 I1 108.95(4) . . ?
I3 Cd1 I6 111.72(5) . 1_655 ?
Cd2 I1 Cd1 104.92(4) . . ?
Cd2 I1 Cs2 137.14(4) . 2_534 ?
Cd1 I1 Cs2 113.66(4) . 2_534 ?
Cd2 I6 Cs1 80.14(3) . . ?
Cd1 I6 Cd2 105.14(4) 1_455 . ?
Cd1 I6 Cs1 84.80(4) 1_455 . ?
Cd1 I2 Cs1 98.32(5) . 1_655 ?
Cd1 I2 Cs2 88.56(4) . . ?
Cs1 I2 Cs2 147.12(4) 1_655 . ?
Cd2 I4 Cs1 87.88(4) . 1_565 ?
Cd2 I4 Cs1 89.40(4) . 2_534 ?
Cd2 I4 Cs2 102.79(4) . 2_544 ?
Cs1 I4 Cs1 140.21(4) 1_565 2_534 ?
Cs2 I4 Cs1 74.78(3) 2_544 2_534 ?
Cs2 I4 Cs1 144.19(4) 2_544 1_565 ?
Cd1 I3 Cs1 111.10(4) . 1_665 ?
Cd1 I3 Cs2 86.69(4) . . ?
Cd1 I3 Cs2 92.79(4) . 2_544 ?
Cs1 I3 Cs2 140.26(4) 1_665 2_544 ?
Cs1 I3 Cs2 78.40(3) 1_665 . ?
Cs2 I3 Cs2 136.27(4) 2_544 . ?
O2 Cs1 I5 72.9(3) . 1_545 ?
O2 Cs1 I5 65.5(3) . . ?
O2 Cs1 I6 91.9(3) . . ?
O2 Cs1 I2 139.5(3) . 1_455 ?
O2 Cs1 I4 63.8(3) . 1_545 ?
O2 Cs1 I4 78.9(3) . 2_535 ?
O2 Cs1 I3 134.7(3) . 1_445 ?
O2 Cs1 Cs2 159.0(3) . 1_445 ?
O2 Cs1 Cs2 35.0(3) . 1_545 ?
O2 Cs1 O1 126.1(4) . 1_445 ?
I5 Cs1 I5 137.18(4) . 1_545 ?
I5 Cs1 I6 65.86(2) . . ?
I5 Cs1 I6 126.64(4) 1_545 . ?
I5 Cs1 I4 101.00(3) . 1_545 ?
I5 Cs1 I4 101.21(3) . 2_535 ?
I5 Cs1 I4 60.12(2) 1_545 2_535 ?
I5 Cs1 Cs2 88.79(3) . 1_545 ?
I5 Cs1 Cs2 129.08(3) . 1_445 ?
I5 Cs1 Cs2 89.05(3) 1_545 1_445 ?
I5 Cs1 Cs2 49.63(2) 1_545 1_545 ?
I6 Cs1 I4 166.62(3) . 2_535 ?
I6 Cs1 Cs2 126.29(3) . 1_545 ?
I6 Cs1 Cs2 107.70(3) . 1_445 ?
I2 Cs1 I5 74.30(3) 1_455 . ?
I2 Cs1 I5 147.50(4) 1_455 1_545 ?
I2 Cs1 I6 66.74(3) 1_455 . ?
I2 Cs1 I4 122.53(4) 1_455 1_545 ?
I2 Cs1 I4 114.47(4) 1_455 2_535 ?
I2 Cs1 I3 70.17(3) 1_455 1_445 ?
I2 Cs1 Cs2 58.71(3) 1_455 1_445 ?
I2 Cs1 Cs2 152.24(4) 1_455 1_545 ?
I4 Cs1 I5 67.56(3) 1_545 1_545 ?
I4 Cs1 I6 60.02(3) 1_545 . ?
I4 Cs1 I4 122.41(3) 1_545 2_535 ?
I4 Cs1 Cs2 81.72(3) 1_545 1_545 ?
I4 Cs1 Cs2 119.53(3) 1_545 1_445 ?
I4 Cs1 Cs2 46.61(2) 2_535 1_545 ?
I4 Cs1 Cs2 82.88(3) 2_535 1_445 ?
I3 Cs1 I5 87.31(3) 1_445 1_545 ?
I3 Cs1 I5 129.54(4) 1_445 . ?
I3 Cs1 I6 67.72(3) 1_445 . ?
I3 Cs1 I4 71.11(3) 1_445 1_545 ?
I3 Cs1 I4 125.61(3) 1_445 2_535 ?
I3 Cs1 Cs2 52.04(2) 1_445 1_445 ?
I3 Cs1 Cs2 135.80(3) 1_445 1_545 ?
Cs2 Cs1 Cs2 124.26(4) 1_545 1_445 ?
O1 Cs1 I5 140.5(3) 1_445 . ?
O1 Cs1 I5 62.2(2) 1_445 1_545 ?
O1 Cs1 I6 138.4(2) 1_445 . ?
O1 Cs1 I2 88.2(2) 1_445 1_455 ?
O1 Cs1 I4 54.1(2) 1_445 2_535 ?
O1 Cs1 I4 118.1(3) 1_445 1_545 ?
O1 Cs1 I3 72.8(2) 1_445 1_445 ?
O1 Cs1 Cs2 91.4(2) 1_445 1_545 ?
O1 Cs1 Cs2 32.9(2) 1_445 1_445 ?
O2 Cs2 I5 74.8(2) 1_565 . ?
O2 Cs2 I1 138.8(2) 1_565 2_535 ?
O2 Cs2 I2 119.9(3) 1_565 . ?
O2 Cs2 I4 89.2(3) 1_565 2_545 ?
O2 Cs2 I3 63.2(3) 1_565 . ?
O2 Cs2 I3 136.5(3) 1_565 2_545 ?
O2 Cs2 Cs1 90.8(2) 1_565 1_665 ?
O2 Cs2 Cs1 33.6(2) 1_565 1_565 ?
I5 Cs2 I1 66.04(3) . 2_535 ?
I5 Cs2 I2 71.67(3) . . ?
I5 Cs2 I3 130.75(4) . 2_545 ?
I5 Cs2 I3 89.06(3) . . ?
I5 Cs2 Cs1 137.58(4) . 1_665 ?
I5 Cs2 Cs1 53.10(2) . 1_565 ?
I1 Cs2 Cs1 107.43(3) 2_535 1_565 ?
I1 Cs2 Cs1 126.86(3) 2_535 1_665 ?
I2 Cs2 I1 59.34(3) . 2_535 ?
I2 Cs2 I3 67.78(3) . . ?
I2 Cs2 Cs1 82.38(3) . 1_665 ?
I2 Cs2 Cs1 121.03(3) . 1_565 ?
I4 Cs2 I5 67.76(3) 2_545 . ?
I4 Cs2 I1 64.95(3) 2_545 2_535 ?
I4 Cs2 I2 120.34(4) 2_545 . ?
I4 Cs2 I3 148.34(4) 2_545 . ?
I4 Cs2 I3 75.05(3) 2_545 2_545 ?
I4 Cs2 Cs1 153.28(4) 2_545 1_665 ?
I4 Cs2 Cs1 58.61(3) 2_545 1_565 ?
I3 Cs2 I1 69.56(3) 2_545 2_535 ?
I3 Cs2 I1 126.12(4) . 2_535 ?
I3 Cs2 I2 102.83(3) 2_545 . ?
I3 Cs2 I3 135.56(4) 2_545 . ?
I3 Cs2 Cs1 86.84(3) 2_545 1_665 ?
I3 Cs2 Cs1 49.56(3) . 1_665 ?
I3 Cs2 Cs1 127.21(4) 2_545 1_565 ?
I3 Cs2 Cs1 90.43(3) . 1_565 ?
Cs1 Cs2 Cs1 124.26(4) 1_565 1_665 ?
O1 Cs2 O2 124.4(3) . 1_565 ?
O1 Cs2 I5 135.6(3) . . ?
O1 Cs2 I1 93.6(2) . 2_535 ?
O1 Cs2 I2 64.1(3) . . ?
O1 Cs2 I4 140.4(3) . 2_545 ?
O1 Cs2 I3 71.2(2) . . ?
O1 Cs2 I3 66.1(3) . 2_545 ?
O1 Cs2 Cs1 157.9(2) . 1_565 ?
O1 Cs2 Cs1 33.8(2) . 1_665 ?
Cs1 O1 H1A 108.9 1_665 . ?
Cs1 O1 H1B 108.9 1_665 . ?
Cs2 O1 Cs1 113.3(4) . 1_665 ?
Cs2 O1 H1A 108.9 . . ?
Cs2 O1 H1B 108.9 . . ?
H1A O1 H1B 107.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
