# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_11
_database_code_depnum_ccdc_archive 'CCDC 1572884'
_audit_update_record             
;
2017-09-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cs O12 P3 Zn4'
_chemical_formula_weight         679.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.488(16)
_cell_length_b                   10.021(11)
_cell_length_c                   16.448(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2388(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1262
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      25.39

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    11.404
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_T_max  1.0000
_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            13665
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         27.52
_reflns_number_total             2729
_reflns_number_gt                1923
_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)+(0.0343P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00034(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2729
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.74913(3) -0.11460(5) 0.92092(4) 0.03311(17) Uani 1 1 d . . .
Zn4 Zn 0.85471(5) 0.12895(7) 0.72562(5) 0.0134(2) Uani 1 1 d . . .
Zn1 Zn 1.04734(6) -0.14782(8) 0.91180(5) 0.0141(2) Uani 1 1 d . . .
Zn3 Zn 0.63364(5) 0.11583(7) 0.69421(5) 0.0129(2) Uani 1 1 d . . .
Zn2 Zn 0.43194(6) -0.14220(7) 0.94397(5) 0.0143(2) Uani 1 1 d . . .
P3 P 0.75650(12) -0.11977(17) 0.65731(11) 0.0118(4) Uani 1 1 d . . .
P1 P 0.94516(12) 0.12857(17) 0.89455(11) 0.0118(4) Uani 1 1 d . . .
P2 P 0.54502(12) 0.10929(17) 0.87473(10) 0.0119(4) Uani 1 1 d . . .
O1 O 0.6156(3) 0.1076(5) 0.8066(3) 0.0215(12) Uani 1 1 d . . .
O2 O 0.8767(3) 0.1846(4) 0.8339(3) 0.0166(11) Uani 1 1 d . . .
O3 O 1.0430(3) 0.1909(5) 0.8811(3) 0.0164(11) Uani 1 1 d . . .
O4 O 0.9118(3) 0.1689(5) 0.9784(3) 0.0219(12) Uani 1 1 d . . .
O5 O 0.5278(3) -0.0298(5) 0.9063(3) 0.0234(12) Uani 1 1 d . . .
O6 O 0.7523(3) -0.2718(4) 0.6763(3) 0.0143(10) Uani 1 1 d . . .
O7 O 0.8036(3) -0.0478(4) 0.7275(3) 0.0186(11) Uani 1 1 d . . .
O8 O 0.8051(3) -0.0972(5) 0.5771(3) 0.0196(11) Uani 1 1 d . . .
O9 O 0.9538(3) -0.0212(5) 0.8833(3) 0.0254(13) Uani 1 1 d . . .
O10 O 0.5786(3) 0.2006(5) 0.9437(3) 0.0175(11) Uani 1 1 d . . .
O11 O 0.4534(3) 0.1780(4) 0.8475(3) 0.0170(11) Uani 1 1 d . . .
O12 O 0.6558(3) -0.0679(4) 0.6510(3) 0.0122(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
Cs1 O2 3.069(5) 8_755 ?
Cs1 O10 3.130(5) 8_755 ?
Cs1 O9 3.170(6) . ?
Cs1 O4 3.322(6) 8_755 ?
Cs1 O5 3.325(6) . ?
Cs1 O7 3.346(6) . ?
Cs1 O8 3.423(5) 2_655 ?
Cs1 O1 3.498(5) . ?
Cs1 O2 3.802(6) . ?
Cs1 P1 3.839(3) 8_755 ?
Cs1 P2 4.138(4) 8_755 ?
Cs1 Zn2 4.230(3) 4_547 ?
Zn4 O2 1.894(5) . ?
Zn4 O7 1.920(5) . ?
Zn4 O11 1.931(5) 6_657 ?
Zn4 O6 2.012(5) 8_765 ?
Zn4 Cs1 4.380(3) 8_765 ?
Zn1 O4 1.913(5) 5_757 ?
Zn1 O9 1.915(5) . ?
Zn1 O11 2.041(5) 8_755 ?
Zn1 O12 2.044(5) 6_657 ?
Zn1 O10 2.431(5) 8_755 ?
Zn1 P2 2.844(3) 8_755 ?
Zn3 O1 1.869(5) . ?
Zn3 O3 1.956(5) 6_557 ?
Zn3 O12 2.000(5) . ?
Zn3 O6 2.021(5) 8_765 ?
Zn2 O5 1.893(5) . ?
Zn2 O8 1.923(5) 6_557 ?
Zn2 O10 1.944(5) 5_657 ?
Zn2 O3 1.999(5) 8_755 ?
Zn2 Cs1 4.230(3) 4_447 ?
Zn2 Cs1 4.295(3) 5_657 ?
P3 O8 1.514(5) . ?
P3 O7 1.523(5) . ?
P3 O12 1.552(5) . ?
P3 O6 1.557(5) . ?
P1 O2 1.515(5) . ?
P1 O4 1.516(5) . ?
P1 O9 1.517(5) . ?
P1 O3 1.565(5) . ?
P1 Cs1 3.839(3) 8_765 ?
P2 O5 1.508(5) . ?
P2 O1 1.517(5) . ?
P2 O10 1.537(5) . ?
P2 O11 1.562(5) . ?
P2 Zn1 2.844(3) 8_765 ?
P2 Cs1 4.138(4) 8_765 ?
O2 Cs1 3.069(5) 8_765 ?
O3 Zn3 1.956(5) 6_657 ?
O3 Zn2 1.999(5) 8_765 ?
O4 Zn1 1.913(5) 5_757 ?
O4 Cs1 3.322(5) 8_765 ?
O6 Zn4 2.012(5) 8_755 ?
O6 Zn3 2.021(5) 8_755 ?
O8 Zn2 1.923(5) 6_657 ?
O8 Cs1 3.423(5) 2_654 ?
O10 Zn2 1.944(5) 5_657 ?
O10 Zn1 2.431(5) 8_765 ?
O10 Cs1 3.130(5) 8_765 ?
O11 Zn4 1.931(5) 6_557 ?
O11 Zn1 2.041(5) 8_765 ?
O12 Zn1 2.044(5) 6_557 ?

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 Cs1 O10 98.15(15) 8_755 8_755 ?
O2 Cs1 O9 131.16(13) 8_755 . ?
O10 Cs1 O9 56.79(14) 8_755 . ?
O2 Cs1 O4 44.57(13) 8_755 8_755 ?
O10 Cs1 O4 98.00(15) 8_755 8_755 ?
O9 Cs1 O4 154.79(13) . 8_755 ?
O2 Cs1 O5 63.97(14) 8_755 . ?
O10 Cs1 O5 158.21(12) 8_755 . ?
O9 Cs1 O5 144.31(13) . . ?
O4 Cs1 O5 60.71(13) 8_755 . ?
O2 Cs1 O7 80.09(12) 8_755 . ?
O10 Cs1 O7 92.53(12) 8_755 . ?
O9 Cs1 O7 62.27(12) . . ?
O4 Cs1 O7 124.53(12) 8_755 . ?
O5 Cs1 O7 96.19(12) . . ?
O2 Cs1 O8 128.30(13) 8_755 2_655 ?
O10 Cs1 O8 117.38(12) 8_755 2_655 ?
O9 Cs1 O8 100.27(13) . 2_655 ?
O4 Cs1 O8 91.73(13) 8_755 2_655 ?
O5 Cs1 O8 70.99(12) . 2_655 ?
O7 Cs1 O8 130.07(13) . 2_655 ?
O2 Cs1 O1 80.68(15) 8_755 . ?
O10 Cs1 O1 151.89(12) 8_755 . ?
O9 Cs1 O1 102.98(14) . . ?
O4 Cs1 O1 100.39(14) 8_755 . ?
O5 Cs1 O1 42.71(11) . . ?
O7 Cs1 O1 59.48(12) . . ?
O8 Cs1 O1 83.20(13) 2_655 . ?
O2 Cs1 O2 129.07(15) 8_755 . ?
O10 Cs1 O2 97.12(14) 8_755 . ?
O9 Cs1 O2 40.45(11) . . ?
O4 Cs1 O2 164.43(11) 8_755 . ?
O5 Cs1 O2 103.88(12) . . ?
O7 Cs1 O2 50.92(10) . . ?
O8 Cs1 O2 84.56(13) 2_655 . ?
O1 Cs1 O2 64.19(13) . . ?
O2 Cs1 P1 21.91(9) 8_755 8_755 ?
O10 Cs1 P1 101.64(13) 8_755 8_755 ?
O9 Cs1 P1 149.52(10) . 8_755 ?
O4 Cs1 P1 23.02(9) 8_755 8_755 ?
O5 Cs1 P1 57.06(11) . 8_755 ?
O7 Cs1 P1 101.52(9) . 8_755 ?
O8 Cs1 P1 109.39(10) 2_655 8_755 ?
O1 Cs1 P1 87.73(11) . 8_755 ?
O2 Cs1 P1 147.43(8) . 8_755 ?
O2 Cs1 P2 84.51(12) 8_755 8_755 ?
O10 Cs1 P2 18.55(9) 8_755 8_755 ?
O9 Cs1 P2 59.17(11) . 8_755 ?
O4 Cs1 P2 96.98(12) 8_755 8_755 ?
O5 Cs1 P2 148.47(9) . 8_755 ?
O7 Cs1 P2 77.82(9) . 8_755 ?
O8 Cs1 P2 135.87(9) 2_655 8_755 ?
O1 Cs1 P2 136.51(9) . 8_755 ?
O2 Cs1 P2 96.19(11) . 8_755 ?
P1 Cs1 P2 93.41(10) 8_755 8_755 ?
O2 Cs1 Zn2 103.84(12) 8_755 4_547 ?
O10 Cs1 Zn2 25.44(9) 8_755 4_547 ?
O9 Cs1 Zn2 71.75(11) . 4_547 ?
O4 Cs1 Zn2 85.05(11) 8_755 4_547 ?
O5 Cs1 Zn2 142.08(9) . 4_547 ?
O7 Cs1 Zn2 117.84(9) . 4_547 ?
O8 Cs1 Zn2 96.13(11) 2_655 4_547 ?
O1 Cs1 Zn2 174.53(8) . 4_547 ?
O2 Cs1 Zn2 110.35(10) . 4_547 ?
P1 Cs1 Zn2 97.60(8) 8_755 4_547 ?
P2 Cs1 Zn2 42.27(6) 8_755 4_547 ?
O2 Zn4 O7 108.8(2) . . ?
O2 Zn4 O11 112.7(2) . 6_657 ?
O7 Zn4 O11 122.0(2) . 6_657 ?
O2 Zn4 O6 111.3(2) . 8_765 ?
O7 Zn4 O6 99.52(19) . 8_765 ?
O11 Zn4 O6 101.1(2) 6_657 8_765 ?
O2 Zn4 Cs1 36.39(14) . 8_765 ?
O7 Zn4 Cs1 113.39(15) . 8_765 ?
O11 Zn4 Cs1 124.16(15) 6_657 8_765 ?
O6 Zn4 Cs1 75.00(15) 8_765 8_765 ?
O4 Zn1 O9 121.6(2) 5_757 . ?
O4 Zn1 O11 113.4(2) 5_757 8_755 ?
O9 Zn1 O11 115.9(2) . 8_755 ?
O4 Zn1 O12 106.4(2) 5_757 6_657 ?
O9 Zn1 O12 99.3(2) . 6_657 ?
O11 Zn1 O12 94.42(18) 8_755 6_657 ?
O4 Zn1 O10 87.66(19) 5_757 8_755 ?
O9 Zn1 O10 86.3(2) . 8_755 ?
O11 Zn1 O10 64.80(17) 8_755 8_755 ?
O12 Zn1 O10 158.59(17) 6_657 8_755 ?
O4 Zn1 P2 104.69(16) 5_757 8_755 ?
O9 Zn1 P2 100.46(17) . 8_755 ?
O11 Zn1 P2 32.28(13) 8_755 8_755 ?
O12 Zn1 P2 126.09(13) 6_657 8_755 ?
O10 Zn1 P2 32.71(11) 8_755 8_755 ?
O1 Zn3 O3 123.3(2) . 6_557 ?
O1 Zn3 O12 109.5(2) . . ?
O3 Zn3 O12 103.69(19) 6_557 . ?
O1 Zn3 O6 106.5(2) . 8_765 ?
O3 Zn3 O6 104.0(2) 6_557 8_765 ?
O12 Zn3 O6 109.23(19) . 8_765 ?
O5 Zn2 O8 120.2(2) . 6_557 ?
O5 Zn2 O10 123.2(2) . 5_657 ?
O8 Zn2 O10 99.6(2) 6_557 5_657 ?
O5 Zn2 O3 101.3(2) . 8_755 ?
O8 Zn2 O3 106.08(19) 6_557 8_755 ?
O10 Zn2 O3 104.7(2) 5_657 8_755 ?
O5 Zn2 Cs1 167.00(16) . 4_447 ?
O8 Zn2 Cs1 68.38(16) 6_557 4_447 ?
O10 Zn2 Cs1 43.78(14) 5_657 4_447 ?
O3 Zn2 Cs1 84.46(15) 8_755 4_447 ?
O5 Zn2 Cs1 105.13(17) . 5_657 ?
O8 Zn2 Cs1 50.86(14) 6_557 5_657 ?
O10 Zn2 Cs1 68.94(15) 5_657 5_657 ?
O3 Zn2 Cs1 151.61(14) 8_755 5_657 ?
Cs1 Zn2 Cs1 71.99(8) 4_447 5_657 ?
O8 P3 O7 112.4(3) . . ?
O8 P3 O12 109.2(3) . . ?
O7 P3 O12 108.3(3) . . ?
O8 P3 O6 109.9(3) . . ?
O7 P3 O6 109.2(3) . . ?
O12 P3 O6 107.7(2) . . ?
O2 P1 O4 106.9(3) . . ?
O2 P1 O9 109.9(3) . . ?
O4 P1 O9 113.6(3) . . ?
O2 P1 O3 110.6(3) . . ?
O4 P1 O3 108.1(3) . . ?
O9 P1 O3 107.7(3) . . ?
O2 P1 Cs1 49.11(18) . 8_765 ?
O4 P1 Cs1 59.0(2) . 8_765 ?
O9 P1 Cs1 137.5(2) . 8_765 ?
O3 P1 Cs1 114.4(2) . 8_765 ?
O5 P2 O1 110.8(3) . . ?
O5 P2 O10 110.4(3) . . ?
O1 P2 O10 109.8(3) . . ?
O5 P2 O11 111.5(3) . . ?
O1 P2 O11 111.5(3) . . ?
O10 P2 O11 102.6(3) . . ?
O5 P2 Zn1 129.7(2) . 8_765 ?
O1 P2 Zn1 119.0(2) . 8_765 ?
O10 P2 Zn1 58.74(19) . 8_765 ?
O11 P2 Zn1 44.27(17) . 8_765 ?
O5 P2 Cs1 132.3(2) . 8_765 ?
O1 P2 Cs1 70.0(2) . 8_765 ?
O10 P2 Cs1 40.39(18) . 8_765 ?
O11 P2 Cs1 111.8(2) . 8_765 ?
Zn1 P2 Cs1 74.19(9) 8_765 8_765 ?
P2 O1 Zn3 145.6(3) . . ?
P2 O1 Cs1 89.0(2) . . ?
Zn3 O1 Cs1 118.8(2) . . ?
P1 O2 Zn4 128.3(3) . . ?
P1 O2 Cs1 109.0(2) . 8_765 ?
Zn4 O2 Cs1 122.1(2) . 8_765 ?
P1 O2 Cs1 77.2(2) . . ?
Zn4 O2 Cs1 92.28(17) . . ?
Cs1 O2 Cs1 93.02(14) 8_765 . ?
P1 O3 Zn3 122.9(3) . 6_657 ?
P1 O3 Zn2 115.2(3) . 8_765 ?
Zn3 O3 Zn2 121.8(2) 6_657 8_765 ?
P1 O4 Zn1 137.0(3) . 5_757 ?
P1 O4 Cs1 98.0(2) . 8_765 ?
Zn1 O4 Cs1 123.9(2) 5_757 8_765 ?
P2 O5 Zn2 141.6(3) . . ?
P2 O5 Cs1 95.9(2) . . ?
Zn2 O5 Cs1 122.1(2) . . ?
P3 O6 Zn4 126.5(2) . 8_755 ?
P3 O6 Zn3 122.8(2) . 8_755 ?
Zn4 O6 Zn3 107.2(2) 8_755 8_755 ?
P3 O7 Zn4 126.7(3) . . ?
P3 O7 Cs1 121.4(2) . . ?
Zn4 O7 Cs1 106.91(17) . . ?
P3 O8 Zn2 124.5(3) . 6_657 ?
P3 O8 Cs1 129.8(2) . 2_654 ?
Zn2 O8 Cs1 103.30(17) 6_657 2_654 ?
P1 O9 Zn1 133.2(3) . . ?
P1 O9 Cs1 101.0(2) . . ?
Zn1 O9 Cs1 114.8(2) . . ?
P2 O10 Zn2 119.8(3) . 5_657 ?
P2 O10 Zn1 88.6(2) . 8_765 ?
Zn2 O10 Zn1 109.5(2) 5_657 8_765 ?
P2 O10 Cs1 121.1(2) . 8_765 ?
Zn2 O10 Cs1 110.78(18) 5_657 8_765 ?
Zn1 O10 Cs1 101.71(17) 8_765 8_765 ?
P2 O11 Zn4 134.1(3) . 6_557 ?
P2 O11 Zn1 103.4(2) . 8_765 ?
Zn4 O11 Zn1 122.5(2) 6_557 8_765 ?
P3 O12 Zn3 115.8(2) . . ?
P3 O12 Zn1 128.7(3) . 6_557 ?
Zn3 O12 Zn1 114.6(2) . 6_557 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.078
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.256
####################################################################### 
# 
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 1572886'
_audit_update_record             
;
2017-09-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'O12 P3 Rb Zn4'
_chemical_formula_weight         631.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.00(3)
_cell_length_b                   9.827(18)
_cell_length_c                   16.04(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2207(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1282
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      25.72

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.089
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2384
_exptl_absorpt_coefficient_mu    13.469
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5316
_exptl_absorpt_correction_T_max  0.6582
_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            13067
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         28.18
_reflns_number_total             2691
_reflns_number_gt                1861
_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)+(0.0000P)²+3.5226P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00069(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2691
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.85462(6) 0.12896(9) 0.72477(6) 0.0180(2) Uani 1 1 d . . .
Zn2 Zn 1.04519(6) -0.14698(9) 0.91230(5) 0.0175(2) Uani 1 1 d . . .
Zn3 Zn 0.63304(6) 0.11806(8) 0.69405(5) 0.0151(2) Uani 1 1 d . . .
Zn4 Zn 1.06666(6) 0.13960(9) 0.44438(6) 0.0183(2) Uani 1 1 d . . .
Rb1 Rb 0.75002(6) -0.11910(10) 0.91026(8) 0.0435(3) Uani 1 1 d . . .
P1 P 0.75587(13) -0.11829(19) 0.65621(13) 0.0163(4) Uani 1 1 d . . .
P2 P 0.94087(13) 0.13206(19) 0.89598(12) 0.0159(4) Uani 1 1 d . . .
P3 P 1.05036(13) 0.11104(19) 0.62488(11) 0.0153(4) Uani 1 1 d . . .
O1 O 0.8702(4) 0.1854(5) 0.8350(3) 0.0205(12) Uani 1 1 d . . .
O2 O 1.0395(3) 0.1935(5) 0.8796(3) 0.0163(11) Uani 1 1 d . . .
O3 O 0.9086(4) 0.1787(6) 0.9794(3) 0.0223(12) Uani 1 1 d . . .
O4 O 1.1231(4) 0.1077(6) 0.6915(3) 0.0251(13) Uani 1 1 d . . .
O5 O 0.9586(3) 0.1783(5) 0.6545(3) 0.0187(11) Uani 1 1 d . . .
O6 O 1.0326(4) -0.0280(5) 0.5915(3) 0.0256(13) Uani 1 1 d . . .
O7 O 1.0829(4) 0.2042(5) 0.5561(3) 0.0229(12) Uani 1 1 d . . .
O8 O 0.6543(3) -0.0658(5) 0.6512(3) 0.0163(11) Uani 1 1 d . . .
O9 O 0.7521(3) -0.2707(5) 0.6731(3) 0.0156(11) Uani 1 1 d . . .
O10 O 0.8038(4) -0.0497(5) 0.7273(3) 0.0228(12) Uani 1 1 d . . .
O11 O 0.8056(4) -0.0913(6) 0.5765(3) 0.0276(13) Uani 1 1 d . . .
O12 O 0.9497(4) -0.0181(5) 0.8882(4) 0.0275(13) 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
Zn1 O1 1.866(6) . ?
Zn1 O10 1.895(6) . ?
Zn1 O5 1.905(5) . ?
Zn1 O9 1.973(5) 8_765 ?
Zn1 Rb1 4.139(5) 8_765 ?
Zn2 O3 1.879(6) 5_757 ?
Zn2 O12 1.881(6) . ?
Zn2 O8 2.002(5) 6_657 ?
Zn2 O5 2.024(6) 3_746 ?
Zn2 O7 2.369(6) 3_746 ?
Zn2 P3 2.793(4) 3_746 ?
Zn3 O4 1.844(6) 6_557 ?
Zn3 O2 1.913(5) 6_557 ?
Zn3 O8 1.956(6) . ?
Zn3 O9 1.973(5) 8_765 ?
Zn4 O6 1.862(6) 5_756 ?
Zn4 O11 1.880(6) 5_756 ?
Zn4 O7 1.915(6) . ?
Zn4 O2 1.978(5) 7_565 ?
Zn4 Rb1 4.201(5) 3_756 ?
Zn4 Rb1 4.300(5) 6_657 ?
Rb1 O1 2.825(6) 8_755 ?
Rb1 O7 2.963(6) 3_746 ?
Rb1 O12 2.988(7) . ?
Rb1 O10 3.106(7) . ?
Rb1 O6 3.173(8) 6_557 ?
Rb1 O3 3.180(7) 8_755 ?
Rb1 O4 3.285(7) 6_557 ?
Rb1 O11 3.463(7) 2_655 ?
Rb1 O4 3.609(7) 3_746 ?
Rb1 P2 3.630(5) 8_755 ?
Rb1 O1 3.638(7) . ?
Rb1 P3 3.640(5) 6_557 ?
P1 O11 1.480(6) . ?
P1 O10 1.485(6) . ?
P1 O8 1.515(5) . ?
P1 O9 1.523(6) . ?
P2 O3 1.485(6) . ?
P2 O12 1.487(6) . ?
P2 O1 1.487(5) . ?
P2 O2 1.530(6) . ?
P2 Rb1 3.630(5) 8_765 ?
P3 O4 1.477(6) . ?
P3 O6 1.488(6) . ?
P3 O7 1.505(6) . ?
P3 O5 1.520(5) . ?
P3 Zn2 2.793(4) 3_756 ?
P3 Rb1 3.640(5) 6_657 ?
P3 Rb1 3.894(5) 3_756 ?
O1 Rb1 2.825(6) 8_765 ?
O2 Zn3 1.913(5) 6_657 ?
O2 Zn4 1.978(5) 7_566 ?
O3 Zn2 1.879(6) 5_757 ?
O3 Rb1 3.180(6) 8_765 ?
O4 Zn3 1.844(6) 6_657 ?
O4 Rb1 3.285(7) 6_657 ?
O4 Rb1 3.609(7) 3_756 ?
O5 Zn2 2.024(6) 3_756 ?
O6 Zn4 1.862(6) 5_756 ?
O6 Rb1 3.173(8) 6_657 ?
O7 Zn2 2.369(6) 3_756 ?
O7 Rb1 2.963(6) 3_756 ?
O8 Zn2 2.002(5) 6_557 ?
O9 Zn3 1.973(5) 8_755 ?
O9 Zn1 1.973(5) 8_755 ?
O11 Zn4 1.880(6) 5_756 ?
O11 Rb1 3.463(7) 2_654 ?

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 Zn1 O10 107.4(2) . . ?
O1 Zn1 O5 113.3(2) . . ?
O10 Zn1 O5 122.4(2) . . ?
O1 Zn1 O9 109.8(2) . 8_765 ?
O10 Zn1 O9 100.8(2) . 8_765 ?
O5 Zn1 O9 101.7(2) . 8_765 ?
O1 Zn1 Rb1 35.15(16) . 8_765 ?
O10 Zn1 Rb1 113.94(18) . 8_765 ?
O5 Zn1 Rb1 122.95(18) . 8_765 ?
O9 Zn1 Rb1 74.63(18) 8_765 8_765 ?
O3 Zn2 O12 123.1(2) 5_757 . ?
O3 Zn2 O8 105.9(2) 5_757 6_657 ?
O12 Zn2 O8 99.7(3) . 6_657 ?
O3 Zn2 O5 110.9(2) 5_757 3_746 ?
O12 Zn2 O5 116.3(2) . 3_746 ?
O8 Zn2 O5 95.1(2) 6_657 3_746 ?
O3 Zn2 O7 87.7(2) 5_757 3_746 ?
O12 Zn2 O7 85.5(3) . 3_746 ?
O8 Zn2 O7 158.83(19) 6_657 3_746 ?
O5 Zn2 O7 64.5(2) 3_746 3_746 ?
O3 Zn2 P3 102.76(18) 5_757 3_746 ?
O12 Zn2 P3 100.9(2) . 3_746 ?
O8 Zn2 P3 126.59(16) 6_657 3_746 ?
O5 Zn2 P3 32.03(15) 3_746 3_746 ?
O7 Zn2 P3 32.59(14) 3_746 3_746 ?
O4 Zn3 O2 125.8(2) 6_557 6_557 ?
O4 Zn3 O8 108.1(2) 6_557 . ?
O2 Zn3 O8 104.2(2) 6_557 . ?
O4 Zn3 O9 105.1(2) 6_557 8_765 ?
O2 Zn3 O9 103.8(2) 6_557 8_765 ?
O8 Zn3 O9 109.1(2) . 8_765 ?
O6 Zn4 O11 120.4(3) 5_756 5_756 ?
O6 Zn4 O7 125.0(2) 5_756 . ?
O11 Zn4 O7 97.9(2) 5_756 . ?
O6 Zn4 O2 100.5(2) 5_756 7_565 ?
O11 Zn4 O2 107.4(2) 5_756 7_565 ?
O7 Zn4 O2 103.9(2) . 7_565 ?
O6 Zn4 Rb1 163.82(17) 5_756 3_756 ?
O11 Zn4 Rb1 70.2(2) 5_756 3_756 ?
O7 Zn4 Rb1 38.81(16) . 3_756 ?
O2 Zn4 Rb1 86.64(19) 7_565 3_756 ?
O6 Zn4 Rb1 105.4(2) 5_756 6_657 ?
O11 Zn4 Rb1 51.65(18) 5_756 6_657 ?
O7 Zn4 Rb1 67.51(19) . 6_657 ?
O2 Zn4 Rb1 152.84(15) 7_565 6_657 ?
Rb1 Zn4 Rb1 70.61(12) 3_756 6_657 ?
O1 Rb1 O7 98.6(2) 8_755 3_746 ?
O1 Rb1 O12 137.11(16) 8_755 . ?
O7 Rb1 O12 58.49(19) 3_746 . ?
O1 Rb1 O10 83.68(17) 8_755 . ?
O7 Rb1 O10 96.28(15) 3_746 . ?
O12 Rb1 O10 65.68(15) . . ?
O1 Rb1 O6 67.45(18) 8_755 6_557 ?
O7 Rb1 O6 157.58(15) 3_746 6_557 ?
O12 Rb1 O6 143.42(18) . 6_557 ?
O10 Rb1 O6 99.32(14) . 6_557 ?
O1 Rb1 O3 46.22(16) 8_755 8_755 ?
O7 Rb1 O3 97.0(2) 3_746 8_755 ?
O12 Rb1 O3 154.48(15) . 8_755 ?
O10 Rb1 O3 129.52(13) . 8_755 ?
O6 Rb1 O3 60.62(17) 6_557 8_755 ?
O1 Rb1 O4 85.8(2) 8_755 6_557 ?
O7 Rb1 O4 156.23(14) 3_746 6_557 ?
O12 Rb1 O4 102.82(18) . 6_557 ?
O10 Rb1 O4 60.82(15) . 6_557 ?
O6 Rb1 O4 44.38(13) 6_557 6_557 ?
O3 Rb1 O4 102.69(19) 8_755 6_557 ?
O1 Rb1 O11 126.94(17) 8_755 2_655 ?
O7 Rb1 O11 112.78(16) 3_746 2_655 ?
O12 Rb1 O11 95.95(16) . 2_655 ?
O10 Rb1 O11 130.63(17) . 2_655 ?
O6 Rb1 O11 67.84(14) 6_557 2_655 ?
O3 Rb1 O11 86.97(17) 8_755 2_655 ?
O4 Rb1 O11 81.72(18) 6_557 2_655 ?
O1 Rb1 O4 66.04(18) 8_755 3_746 ?
O7 Rb1 O4 42.10(14) 3_746 3_746 ?
O12 Rb1 O4 74.51(17) . 3_746 ?
O10 Rb1 O4 67.45(15) . 3_746 ?
O6 Rb1 O4 132.66(14) 6_557 3_746 ?
O3 Rb1 O4 92.11(18) 8_755 3_746 ?
O4 Rb1 O4 123.09(19) 6_557 3_746 ?
O11 Rb1 O4 154.57(12) 2_655 3_746 ?
O1 Rb1 P2 22.52(11) 8_755 8_755 ?
O7 Rb1 P2 101.42(18) 3_746 8_755 ?
O12 Rb1 P2 154.85(12) . 8_755 ?
O10 Rb1 P2 105.47(11) . 8_755 ?
O6 Rb1 P2 58.87(15) 6_557 8_755 ?
O3 Rb1 P2 24.05(11) 8_755 8_755 ?
O4 Rb1 P2 91.58(16) 6_557 8_755 ?
O11 Rb1 P2 106.56(13) 2_655 8_755 ?
O4 Rb1 P2 80.37(16) 3_746 8_755 ?
O1 Rb1 O1 133.86(19) 8_755 . ?
O7 Rb1 O1 100.21(18) 3_746 . ?
O12 Rb1 O1 41.84(13) . . ?
O10 Rb1 O1 52.69(12) . . ?
O6 Rb1 O1 102.04(16) 6_557 . ?
O3 Rb1 O1 162.27(13) 8_755 . ?
O4 Rb1 O1 61.78(17) 6_557 . ?
O11 Rb1 O1 82.45(17) 2_655 . ?
O4 Rb1 O1 103.53(18) 3_746 . ?
P2 Rb1 O1 150.86(10) 8_755 . ?
O1 Rb1 P3 84.20(17) 8_755 6_557 ?
O7 Rb1 P3 177.17(11) 3_746 6_557 ?
O12 Rb1 P3 119.61(16) . 6_557 ?
O10 Rb1 P3 84.46(12) . 6_557 ?
O6 Rb1 P3 24.00(10) 6_557 6_557 ?
O3 Rb1 P3 84.60(17) 8_755 6_557 ?
O4 Rb1 P3 23.93(10) 6_557 6_557 ?
O11 Rb1 P3 64.89(12) 2_655 6_557 ?
O4 Rb1 P3 140.35(11) 3_746 6_557 ?
P2 Rb1 P3 80.98(15) 8_755 6_557 ?
O1 Rb1 P3 78.04(15) . 6_557 ?
O11 P1 O10 111.7(3) . . ?
O11 P1 O8 109.6(3) . . ?
O10 P1 O8 108.1(3) . . ?
O11 P1 O9 110.3(3) . . ?
O10 P1 O9 109.0(3) . . ?
O8 P1 O9 108.2(3) . . ?
O3 P2 O12 114.1(3) . . ?
O3 P2 O1 106.4(3) . . ?
O12 P2 O1 110.5(3) . . ?
O3 P2 O2 107.9(3) . . ?
O12 P2 O2 107.6(3) . . ?
O1 P2 O2 110.4(3) . . ?
O3 P2 Rb1 60.7(2) . 8_765 ?
O12 P2 Rb1 137.4(2) . 8_765 ?
O1 P2 Rb1 46.7(2) . 8_765 ?
O2 P2 Rb1 114.2(2) . 8_765 ?
O4 P3 O6 110.8(3) . . ?
O4 P3 O7 109.6(3) . . ?
O6 P3 O7 110.2(3) . . ?
O4 P3 O5 111.5(3) . . ?
O6 P3 O5 111.8(3) . . ?
O7 P3 O5 102.7(3) . . ?
O4 P3 Zn2 120.2(2) . 3_756 ?
O6 P3 Zn2 128.7(2) . 3_756 ?
O7 P3 Zn2 58.0(2) . 3_756 ?
O5 P3 Zn2 44.9(2) . 3_756 ?
O4 P3 Rb1 64.4(2) . 6_657 ?
O6 P3 Rb1 60.1(2) . 6_657 ?
O7 P3 Rb1 91.8(2) . 6_657 ?
O5 P3 Rb1 165.3(2) . 6_657 ?
Zn2 P3 Rb1 149.75(8) 3_756 6_657 ?
O4 P3 Rb1 67.9(2) . 3_756 ?
O6 P3 Rb1 133.9(2) . 3_756 ?
O7 P3 Rb1 42.4(2) . 3_756 ?
O5 P3 Rb1 110.8(2) . 3_756 ?
Zn2 P3 Rb1 74.51(14) 3_756 3_756 ?
Rb1 P3 Rb1 81.34(15) 6_657 3_756 ?
P2 O1 Zn1 126.6(3) . . ?
P2 O1 Rb1 110.8(3) . 8_765 ?
Zn1 O1 Rb1 122.5(2) . 8_765 ?
P2 O1 Rb1 78.5(2) . . ?
Zn1 O1 Rb1 90.9(2) . . ?
Rb1 O1 Rb1 98.17(19) 8_765 . ?
P2 O2 Zn3 124.8(3) . 6_657 ?
P2 O2 Zn4 114.2(3) . 7_566 ?
Zn3 O2 Zn4 120.9(3) 6_657 7_566 ?
P2 O3 Zn2 132.6(4) . 5_757 ?
P2 O3 Rb1 95.2(3) . 8_765 ?
Zn2 O3 Rb1 131.8(2) 5_757 8_765 ?
P3 O4 Zn3 140.4(4) . 6_657 ?
P3 O4 Rb1 91.6(3) . 6_657 ?
Zn3 O4 Rb1 119.4(2) 6_657 6_657 ?
P3 O4 Rb1 89.8(3) . 3_756 ?
Zn3 O4 Rb1 111.9(2) 6_657 3_756 ?
Rb1 O4 Rb1 90.79(18) 6_657 3_756 ?
P3 O5 Zn1 136.0(3) . . ?
P3 O5 Zn2 103.1(3) . 3_756 ?
Zn1 O5 Zn2 120.6(2) . 3_756 ?
P3 O6 Zn4 141.0(4) . 5_756 ?
P3 O6 Rb1 95.9(2) . 6_657 ?
Zn4 O6 Rb1 123.2(3) 5_756 6_657 ?
P3 O7 Zn4 116.7(3) . . ?
P3 O7 Zn2 89.4(3) . 3_756 ?
Zn4 O7 Zn2 108.4(2) . 3_756 ?
P3 O7 Rb1 117.5(3) . 3_756 ?
Zn4 O7 Rb1 117.3(2) . 3_756 ?
Zn2 O7 Rb1 101.4(2) 3_756 3_756 ?
P1 O8 Zn3 116.0(3) . . ?
P1 O8 Zn2 127.4(3) . 6_557 ?
Zn3 O8 Zn2 115.5(2) . 6_557 ?
P1 O9 Zn3 123.2(3) . 8_755 ?
P1 O9 Zn1 126.3(3) . 8_755 ?
Zn3 O9 Zn1 105.6(3) 8_755 8_755 ?
P1 O10 Zn1 125.0(3) . . ?
P1 O10 Rb1 121.1(3) . . ?
Zn1 O10 Rb1 108.4(2) . . ?
P1 O11 Zn4 123.8(3) . 5_756 ?
P1 O11 Rb1 131.8(3) . 2_654 ?
Zn4 O11 Rb1 103.2(2) 5_756 2_654 ?
P2 O12 Zn2 135.3(3) . . ?
P2 O12 Rb1 104.0(3) . . ?
Zn2 O12 Rb1 114.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.18
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.268
####################################################################### 
# 
# 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_333
_database_code_depnum_ccdc_archive 'CCDC 1572885'
_audit_update_record             
;
2017-09-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Cs O11 P2 Zn4'
_chemical_formula_weight         643.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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)/m  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.048(3)
_cell_length_b                   14.368(8)
_cell_length_c                   8.111(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.797(6)
_cell_angle_gamma                90.00
_cell_volume                     560.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1663
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      27.66

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.068
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             596
_exptl_absorpt_coefficient_mu    11.999
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5110
_exptl_absorpt_correction_T_max  0.7456
_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            3470
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         27.69
_reflns_number_total             1351
_reflns_number_gt                1207
_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)+(0.0230P)²+0.9532P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1351
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0498
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.17935(8) 0.2500 0.84063(6) 0.03354(12) Uani 1 2 d S . .
Zn1 Zn 0.19685(8) 0.55893(3) 0.82258(5) 0.01276(11) Uani 1 1 d . . .
Zn2 Zn 0.40637(8) 0.35609(3) 0.38809(5) 0.01169(11) Uani 1 1 d . . .
P1 P 0.66229(18) 0.43777(6) 0.76915(12) 0.01117(19) Uani 1 1 d . . .
B1 B 0.1314(10) 0.7500 0.6892(7) 0.0090(10) Uani 1 2 d S . .
O1 O 0.5096(5) 0.53400(17) 0.7299(3) 0.0171(5) Uani 1 1 d . . .
O2 O 0.6398(6) 0.40213(18) 0.9417(3) 0.0228(6) Uani 1 1 d . . .
O3 O 0.5194(6) 0.36603(18) 0.6335(3) 0.0202(6) Uani 1 1 d . . .
O4 O 0.9606(5) 0.45256(18) 0.7723(4) 0.0261(7) Uani 1 1 d . . .
O5 O 0.4038(7) 0.7500 0.6846(4) 0.0132(7) Uani 1 2 d S . .
O6 O -0.0020(5) 0.66690(16) 0.6930(3) 0.0143(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
Cs1 O4 3.102(3) 4_465 ?
Cs1 O4 3.102(3) 1_455 ?
Cs1 O2 3.112(3) 4_565 ?
Cs1 O2 3.112(3) . ?
Cs1 O3 3.211(3) 4_565 ?
Cs1 O3 3.211(3) . ?
Cs1 O3 3.644(3) 4_465 ?
Cs1 O3 3.644(3) 1_455 ?
Cs1 P1 3.6746(17) 4_465 ?
Cs1 P1 3.6746(17) 1_455 ?
Cs1 O2 3.773(3) 4_465 ?
Cs1 O2 3.773(3) 1_455 ?
Zn1 O4 1.904(3) 1_455 ?
Zn1 O2 1.919(3) 3_667 ?
Zn1 O6 1.968(2) . ?
Zn1 O1 1.978(3) . ?
Zn1 Cs1 4.4335(15) 3_667 ?
Zn2 O3 1.901(3) . ?
Zn2 O1 1.959(3) 3_666 ?
Zn2 O6 1.972(3) 3_566 ?
Zn2 O5 1.983(2) 3_666 ?
Zn2 Zn2 3.0486(18) 4_565 ?
P1 O4 1.513(3) . ?
P1 O3 1.519(3) . ?
P1 O2 1.527(3) . ?
P1 O1 1.567(3) . ?
P1 Cs1 3.6746(17) 1_655 ?
B1 O6 1.376(3) 4_575 ?
B1 O6 1.376(3) . ?
B1 O5 1.387(6) . ?
O1 Zn2 1.959(3) 3_666 ?
O2 Zn1 1.919(3) 3_667 ?
O2 Cs1 3.773(3) 1_655 ?
O3 Cs1 3.644(3) 1_655 ?
O4 Zn1 1.904(3) 1_655 ?
O4 Cs1 3.102(3) 1_655 ?
O5 Zn2 1.983(2) 2_656 ?
O5 Zn2 1.983(2) 3_666 ?
O5 Cs1 3.782(4) 3_667 ?
O6 Zn2 1.972(3) 3_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cs1 O4 139.52(10) 4_465 1_455 ?
O4 Cs1 O2 65.45(8) 4_465 4_565 ?
O4 Cs1 O2 154.46(7) 1_455 4_565 ?
O4 Cs1 O2 154.46(7) 4_465 . ?
O4 Cs1 O2 65.45(8) 1_455 . ?
O2 Cs1 O2 89.22(11) 4_565 . ?
O4 Cs1 O3 68.74(7) 4_465 4_565 ?
O4 Cs1 O3 127.71(8) 1_455 4_565 ?
O2 Cs1 O3 45.38(7) 4_565 4_565 ?
O2 Cs1 O3 91.54(8) . 4_565 ?
O4 Cs1 O3 127.71(8) 4_465 . ?
O4 Cs1 O3 68.74(7) 1_455 . ?
O2 Cs1 O3 91.54(8) 4_565 . ?
O2 Cs1 O3 45.38(7) . . ?
O3 Cs1 O3 62.56(10) 4_565 . ?
O4 Cs1 O3 42.53(6) 4_465 4_465 ?
O4 Cs1 O3 96.98(7) 1_455 4_465 ?
O2 Cs1 O3 107.70(7) 4_565 4_465 ?
O2 Cs1 O3 161.20(6) . 4_465 ?
O3 Cs1 O3 94.64(7) 4_565 4_465 ?
O3 Cs1 O3 123.78(8) . 4_465 ?
O4 Cs1 O3 96.98(7) 4_465 1_455 ?
O4 Cs1 O3 42.53(6) 1_455 1_455 ?
O2 Cs1 O3 161.20(7) 4_565 1_455 ?
O2 Cs1 O3 107.70(7) . 1_455 ?
O3 Cs1 O3 123.78(8) 4_565 1_455 ?
O3 Cs1 O3 94.64(7) . 1_455 ?
O3 Cs1 O3 54.45(9) 4_465 1_455 ?
O4 Cs1 P1 23.95(5) 4_465 4_465 ?
O4 Cs1 P1 117.63(6) 1_455 4_465 ?
O2 Cs1 P1 87.89(7) 4_565 4_465 ?
O2 Cs1 P1 173.95(5) . 4_465 ?
O3 Cs1 P1 90.22(6) 4_565 4_465 ?
O3 Cs1 P1 140.01(5) . 4_465 ?
O3 Cs1 P1 23.96(4) 4_465 4_465 ?
O3 Cs1 P1 75.99(6) 1_455 4_465 ?
O4 Cs1 P1 117.63(6) 4_465 1_455 ?
O4 Cs1 P1 23.95(5) 1_455 1_455 ?
O2 Cs1 P1 173.95(5) 4_565 1_455 ?
O2 Cs1 P1 87.89(7) . 1_455 ?
O3 Cs1 P1 140.01(5) 4_565 1_455 ?
O3 Cs1 P1 90.22(6) . 1_455 ?
O3 Cs1 P1 75.99(6) 4_465 1_455 ?
O3 Cs1 P1 23.96(4) 1_455 1_455 ?
P1 Cs1 P1 94.48(5) 4_465 1_455 ?
O4 Cs1 O2 41.76(7) 4_465 4_465 ?
O4 Cs1 O2 109.95(7) 1_455 4_465 ?
O2 Cs1 O2 93.82(8) 4_565 4_465 ?
O2 Cs1 O2 151.67(9) . 4_465 ?
O3 Cs1 O2 110.47(7) 4_565 4_465 ?
O3 Cs1 O2 162.06(6) . 4_465 ?
O3 Cs1 O2 38.38(6) 4_465 4_465 ?
O3 Cs1 O2 75.30(7) 1_455 4_465 ?
P1 Cs1 O2 23.61(4) 4_465 4_465 ?
P1 Cs1 O2 86.24(6) 1_455 4_465 ?
O4 Cs1 O2 109.95(7) 4_465 1_455 ?
O4 Cs1 O2 41.76(7) 1_455 1_455 ?
O2 Cs1 O2 151.67(9) 4_565 1_455 ?
O2 Cs1 O2 93.82(8) . 1_455 ?
O3 Cs1 O2 162.06(6) 4_565 1_455 ?
O3 Cs1 O2 110.47(7) . 1_455 ?
O3 Cs1 O2 75.30(7) 4_465 1_455 ?
O3 Cs1 O2 38.38(6) 1_455 1_455 ?
P1 Cs1 O2 86.24(6) 4_465 1_455 ?
P1 Cs1 O2 23.61(4) 1_455 1_455 ?
O2 Cs1 O2 70.81(9) 4_465 1_455 ?
O4 Zn1 O2 119.83(13) 1_455 3_667 ?
O4 Zn1 O6 109.53(12) 1_455 . ?
O2 Zn1 O6 107.21(11) 3_667 . ?
O4 Zn1 O1 107.08(12) 1_455 . ?
O2 Zn1 O1 106.34(12) 3_667 . ?
O6 Zn1 O1 106.03(11) . . ?
O4 Zn1 Cs1 155.39(10) 1_455 3_667 ?
O2 Zn1 Cs1 36.66(8) 3_667 3_667 ?
O6 Zn1 Cs1 89.50(8) . 3_667 ?
O1 Zn1 Cs1 81.20(8) . 3_667 ?
O4 Zn1 Cs1 35.69(8) 1_455 . ?
O2 Zn1 Cs1 105.38(8) 3_667 . ?
O6 Zn1 Cs1 142.46(7) . . ?
O1 Zn1 Cs1 81.82(7) . . ?
Cs1 Zn1 Cs1 128.01(2) 3_667 . ?
O3 Zn2 O1 114.24(11) . 3_666 ?
O3 Zn2 O6 108.10(11) . 3_566 ?
O1 Zn2 O6 109.19(10) 3_666 3_566 ?
O3 Zn2 O5 110.56(13) . 3_666 ?
O1 Zn2 O5 106.14(11) 3_666 3_666 ?
O6 Zn2 O5 108.48(12) 3_566 3_666 ?
O3 Zn2 Zn2 94.31(8) . 4_565 ?
O1 Zn2 Zn2 143.71(8) 3_666 4_565 ?
O6 Zn2 Zn2 80.36(7) 3_566 4_565 ?
O5 Zn2 Zn2 39.78(8) 3_666 4_565 ?
O3 Zn2 Cs1 39.67(8) . . ?
O1 Zn2 Cs1 146.15(8) 3_666 . ?
O6 Zn2 Cs1 73.47(8) 3_566 . ?
O5 Zn2 Cs1 104.60(9) 3_666 . ?
Zn2 Zn2 Cs1 69.904(14) 4_565 . ?
O4 P1 O3 110.94(16) . . ?
O4 P1 O2 112.58(17) . . ?
O3 P1 O2 106.51(15) . . ?
O4 P1 O1 107.73(15) . . ?
O3 P1 O1 110.88(15) . . ?
O2 P1 O1 108.19(15) . . ?
O4 P1 Cs1 56.30(11) . 1_655 ?
O3 P1 Cs1 76.90(11) . 1_655 ?
O2 P1 Cs1 81.80(12) . 1_655 ?
O1 P1 Cs1 163.97(10) . 1_655 ?
O4 P1 Cs1 141.18(11) . . ?
O3 P1 Cs1 56.19(11) . . ?
O2 P1 Cs1 52.46(10) . . ?
O1 P1 Cs1 111.03(10) . . ?
Cs1 P1 Cs1 84.98(5) 1_655 . ?
O6 B1 O6 120.4(4) 4_575 . ?
O6 B1 O5 119.8(2) 4_575 . ?
O6 B1 O5 119.8(2) . . ?
P1 O1 Zn2 130.07(15) . 3_666 ?
P1 O1 Zn1 118.87(14) . . ?
Zn2 O1 Zn1 110.90(12) 3_666 . ?
P1 O2 Zn1 133.28(17) . 3_667 ?
P1 O2 Cs1 104.65(13) . . ?
Zn1 O2 Cs1 121.74(11) 3_667 . ?
P1 O2 Cs1 74.59(11) . 1_655 ?
Zn1 O2 Cs1 105.45(11) 3_667 1_655 ?
Cs1 O2 Cs1 93.82(8) . 1_655 ?
P1 O3 Zn2 137.16(17) . . ?
P1 O3 Cs1 100.66(13) . . ?
Zn2 O3 Cs1 118.13(11) . . ?
P1 O3 Cs1 79.15(11) . 1_655 ?
Zn2 O3 Cs1 112.81(11) . 1_655 ?
Cs1 O3 Cs1 94.64(7) . 1_655 ?
P1 O4 Zn1 132.15(17) . 1_655 ?
P1 O4 Cs1 99.75(13) . 1_655 ?
Zn1 O4 Cs1 123.32(12) 1_655 1_655 ?
B1 O5 Zn2 125.52(13) . 2_656 ?
B1 O5 Zn2 125.52(13) . 3_666 ?
Zn2 O5 Zn2 100.45(15) 2_656 3_666 ?
B1 O5 Cs1 102.7(3) . 3_667 ?
Zn2 O5 Cs1 97.68(11) 2_656 3_667 ?
Zn2 O5 Cs1 97.68(11) 3_666 3_667 ?
B1 O6 Zn1 121.5(2) . . ?
B1 O6 Zn2 127.0(2) . 3_566 ?
Zn1 O6 Zn2 110.69(12) . 3_566 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.69
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.145
