 
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         
;         
Dicaesium Diaquatrinickel 24-oxodihydroxotetraborohexaphosphate(V)
;
_chemical_name_common             'Caesium nickel borophosphate'
_chemical_melting_point           ?
_chemical_formula_moiety          'B8 H12 Ni6 O56 P12, 4(Cs)'
_chemical_formula_sum
 'B8 Cs4 H12 Ni6 O56 P12'
_chemical_formula_weight          2250.12

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'
 'B'  'B'   0.0013   0.0007
 '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'
 'Ni'  'Ni'   0.3393   1.1124
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            61
_space_group_name_H-M_alt         'P b c a'
_space_group_name_Hall            '-P 2ac 2ab'
 
_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.
;
 
loop_
 _space_group_symop_operation_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                    9.5200(4)
_cell_length_b                    12.2546(5)
_cell_length_c                    19.9660(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2329.31(15)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     6262
_cell_measurement_theta_min       2.8920
_cell_measurement_theta_max       29.4490
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             green
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.208          
_exptl_crystal_F_000              2136
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.093
_exptl_crystal_size_mid           0.056
_exptl_crystal_size_min           0.028
_exptl_absorpt_coefficient_mu     6.022
_shelx_estimated_absorpt_T_min    0.604
_shelx_estimated_absorpt_T_max    0.849
_exptl_absorpt_correction_type    'gaussian'
_exptl_absorpt_correction_T_min   0.600
_exptl_absorpt_correction_T_max   0.716
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type   'Xcalibur, Sapphire3'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  16.0630
_diffrn_reflns_number             36893
_diffrn_reflns_av_unetI/netI      0.0490
_diffrn_reflns_av_R_equivalents   0.1160
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          2.895
_diffrn_reflns_theta_max          27.496
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              2670
_reflns_number_gt                 2423
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution     'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'DIMOND (Brandenburg, 2006)'
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0238P)²+15.1911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.00047(10)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2670
_refine_ls_number_parameters      197
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.0781
_refine_ls_R_factor_gt            0.0662
_refine_ls_wR_factor_ref          0.1033
_refine_ls_wR_factor_gt           0.0996
_refine_ls_goodness_of_fit_ref    1.299
_refine_ls_restrained_S_all       1.298
_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_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
Cs1 Cs 0.3498(3) 0.0896(2) 0.14664(11) 0.0297(4) Uani 0.62 1 d . . P . .
Cs2 Cs 0.3042(4) 0.1071(4) 0.1583(3) 0.0297(4) Uani 0.22 1 d . . P . .
Cs3 Cs 0.3347(13) 0.1047(10) 0.1352(5) 0.0297(4) Uani 0.16 1 d . . P . .
Ni1 Ni 0.68817(8) 0.31233(6) 0.08157(4) 0.00351(19) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.0000 0.5000 0.0090(3) Uani 1 2 d S . P . .
P1 P 0.51497(16) 0.34053(13) 0.21681(8) 0.0029(3) Uani 1 1 d . . . . .
P2 P 0.27411(17) 0.06351(13) 0.37742(8) 0.0036(3) Uani 1 1 d . . . . .
P3 P 0.51049(17) 0.27543(14) 0.45528(9) 0.0070(4) Uani 1 1 d . . . . .
O5 O 0.3832(4) 0.4094(3) 0.2305(2) 0.0053(6) Uani 1 1 d . . . . .
O1 O 0.5158(4) 0.3101(3) 0.1437(2) 0.0054(9) Uani 1 1 d . . . . .
O2 O 0.5659(5) 0.1759(4) 0.4937(2) 0.0089(10) Uani 1 1 d . . . . .
O3 O 0.5034(5) 0.2385(3) 0.2617(2) 0.0053(6) Uani 1 1 d . . . . .
O4 O 0.3098(4) 0.3064(4) 0.3294(2) 0.0066(9) Uani 1 1 d . . . . .
O6 O 0.6441(4) 0.4087(4) 0.2370(2) 0.0069(9) Uani 1 1 d . . . . .
O7 O 0.5347(4) 0.2600(4) 0.3789(2) 0.0096(7) Uani 1 1 d . . . . .
O8 O 0.3618(5) 0.3035(4) 0.4733(2) 0.0130(10) Uani 1 1 d . . . . .
O9 O 0.1781(5) 0.0012(4) 0.3287(2) 0.0096(7) Uani 1 1 d . . . . .
O10 O 0.1817(5) 0.1452(4) 0.4126(2) 0.0084(9) Uani 1 1 d . . . . .
O11 O 0.3425(5) -0.0170(4) 0.4259(2) 0.0071(9) Uani 1 1 d . . . . .
O12 O 0.3875(5) 0.1203(4) 0.3354(3) 0.0132(11) Uani 1 1 d . . . . .
O13 O 0.6090(5) 0.3756(4) 0.4694(2) 0.0139(11) Uani 1 1 d D . . . .
O14 O 0.3626(5) 0.0481(4) 0.5694(2) 0.0124(10) Uani 1 1 d D . . . .
B1 B 0.4300(7) 0.2340(6) 0.3276(4) 0.0040(10) Uani 1 1 d . . . . .
B2 B 0.2908(7) 0.4024(6) 0.2894(4) 0.0040(10) Uani 1 1 d . . . . .
H1 H 0.278(4) 0.075(6) 0.555(4) 0.02(2) Uiso 1 1 d D . . . .
H2 H 0.394(13) 0.105(7) 0.595(6) 0.10(5) Uiso 1 1 d D . . . .
H3 H 0.638(12) 0.366(10) 0.513(2) 0.08(4) Uiso 1 1 d 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 Cs2 0.537(5) . ?
Cs1 O14 3.051(6) 2_554 ?
Cs1 O1 3.131(5) . ?
Cs1 O6 3.212(5) 3_645 ?
Cs1 O3 3.278(5) . ?
Cs1 O9 3.345(5) 6_656 ?
Cs1 O10 3.442(5) 6_656 ?
Cs1 O13 3.520(6) 3_645 ?
Cs1 O5 3.549(5) 8_655 ?
Cs1 O7 3.690(5) 6_556 ?
Cs1 O8 3.702(5) 7_565 ?
Cs1 P1 3.727(3) . ?
Cs2 Cs3 0.546(14) . ?
Cs2 O14 3.048(7) 2_554 ?
Cs2 O1 3.214(6) . ?
Cs2 O3 3.232(7) . ?
Cs2 O6 3.243(7) 3_645 ?
Cs2 O7 3.263(6) 6_556 ?
Cs2 O5 3.335(6) 8_655 ?
Cs2 O12 3.627(7) . ?
Cs2 O3 3.653(6) 6_556 ?
Cs2 P1 3.684(5) . ?
Cs2 B2 3.735(9) 8_655 ?
Cs3 O14 2.960(13) 2_554 ?
Cs3 O1 3.055(12) . ?
Cs3 O3 3.412(13) . ?
Cs3 O8 3.433(11) 7_565 ?
Cs3 O7 3.444(13) 6_556 ?
Cs3 O10 3.474(14) 6_656 ?
Cs3 O6 3.510(10) 3_645 ?
Cs3 O13 3.539(14) 3_645 ?
Cs3 O9 3.580(13) 6_656 ?
Cs3 O5 3.694(12) 8_655 ?
Cs3 O2 3.733(11) 6_556 ?
Ni1 O8 1.986(5) 6_656 ?
Ni1 O10 2.052(4) 6_656 ?
Ni1 O1 2.058(4) . ?
Ni1 O2 2.110(4) 7_565 ?
Ni1 O11 2.117(4) 3_655 ?
Ni1 O4 2.122(4) 6_656 ?
Ni2 O14 1.995(5) 5_656 ?
Ni2 O14 1.995(5) . ?
Ni2 O11 2.116(4) 5_656 ?
Ni2 O11 2.116(4) . ?
Ni2 O2 2.249(5) 5_656 ?
Ni2 O2 2.249(5) . ?
Ni2 Cs3 4.369(11) 6_656 ?
Ni2 Cs3 4.369(11) 2 ?
P1 O1 1.506(4) . ?
P1 O5 1.537(4) . ?
P1 O6 1.540(5) . ?
P1 O3 1.541(4) . ?
P2 O10 1.507(5) . ?
P2 O11 1.528(5) . ?
P2 O12 1.534(5) . ?
P2 O9 1.538(5) . ?
P2 Cs1 4.081(4) 6_556 ?
P2 Cs3 4.221(13) 6_556 ?
P3 O8 1.501(5) . ?
P3 O2 1.535(5) . ?
P3 O7 1.555(5) . ?
P3 O13 1.571(5) . ?
P3 Cs3 4.144(11) 6_656 ?
P3 Cs2 4.150(5) 6_656 ?
P3 Cs3 4.227(11) 7_566 ?
O5 B2 1.470(8) . ?
O5 Cs2 3.336(6) 8_665 ?
O5 Cs1 3.549(5) 8_665 ?
O5 Cs3 3.694(12) 8_665 ?
O2 Ni1 2.110(4) 7_566 ?
O2 Cs3 3.733(11) 6_656 ?
O3 B1 1.492(8) . ?
O3 Cs2 3.653(6) 6_656 ?
O4 B2 1.433(8) . ?
O4 B1 1.448(8) . ?
O4 Ni1 2.122(4) 6_556 ?
O6 B2 1.495(8) 6_656 ?
O6 Cs1 3.212(5) 3_655 ?
O6 Cs2 3.243(7) 3_655 ?
O6 Cs3 3.510(10) 3_655 ?
O7 B1 1.464(8) . ?
O7 Cs2 3.263(6) 6_656 ?
O7 Cs3 3.444(13) 6_656 ?
O7 Cs1 3.690(5) 6_656 ?
O8 Ni1 1.986(5) 6_556 ?
O8 Cs3 3.433(11) 7_566 ?
O8 Cs1 3.702(5) 7_566 ?
O9 B2 1.473(8) 8_655 ?
O9 Cs1 3.345(5) 6_556 ?
O9 Cs3 3.580(13) 6_556 ?
O9 Cs2 3.797(6) 6_556 ?
O10 Ni1 2.052(4) 6_556 ?
O10 Cs1 3.442(5) 6_556 ?
O10 Cs3 3.474(14) 6_556 ?
O11 Ni1 2.117(4) 3_645 ?
O12 B1 1.459(8) . ?
O13 Cs1 3.520(6) 3_655 ?
O13 Cs3 3.539(14) 3_655 ?
O13 H3 0.920(10) . ?
O14 Cs3 2.960(13) 2 ?
O14 Cs2 3.048(7) 2 ?
O14 Cs1 3.051(6) 2 ?
O14 H1 0.917(10) . ?
O14 H2 0.919(10) . ?
B1 Cs2 3.898(8) 6_656 ?
B2 O9 1.473(8) 8_665 ?
B2 O6 1.495(8) 6_556 ?
B2 Cs2 3.735(9) 8_665 ?
B2 Cs1 3.895(7) 8_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
Cs2 Cs1 O14 84.6(7) . 2_554 ?
Cs2 Cs1 O1 94.1(7) . . ?
O14 Cs1 O1 143.34(14) 2_554 . ?
Cs2 Cs1 O6 88.6(7) . 3_645 ?
O14 Cs1 O6 89.77(14) 2_554 3_645 ?
O1 Cs1 O6 126.87(14) . 3_645 ?
Cs2 Cs1 O3 80.4(7) . . ?
O14 Cs1 O3 163.25(16) 2_554 . ?
O1 Cs1 O3 46.14(12) . . ?
O6 Cs1 O3 82.51(12) 3_645 . ?
Cs2 Cs1 O9 145.0(8) . 6_656 ?
O14 Cs1 O9 120.96(16) 2_554 6_656 ?
O1 Cs1 O9 79.08(13) . 6_656 ?
O6 Cs1 O9 69.69(12) 3_645 6_656 ?
O3 Cs1 O9 70.14(12) . 6_656 ?
Cs2 Cs1 O10 144.2(7) . 6_656 ?
O14 Cs1 O10 122.96(15) 2_554 6_656 ?
O1 Cs1 O10 50.16(12) . 6_656 ?
O6 Cs1 O10 111.63(13) 3_645 6_656 ?
O3 Cs1 O10 73.78(12) . 6_656 ?
O9 Cs1 O10 42.00(11) 6_656 6_656 ?
Cs2 Cs1 O13 132.3(8) . 3_645 ?
O14 Cs1 O13 47.91(13) 2_554 3_645 ?
O1 Cs1 O13 125.05(14) . 3_645 ?
O6 Cs1 O13 87.70(13) 3_645 3_645 ?
O3 Cs1 O13 145.68(15) . 3_645 ?
O9 Cs1 O13 75.61(13) 6_656 3_645 ?
O10 Cs1 O13 79.58(13) 6_656 3_645 ?
Cs2 Cs1 O5 62.5(7) . 8_655 ?
O14 Cs1 O5 58.71(13) 2_554 8_655 ?
O1 Cs1 O5 149.42(14) . 8_655 ?
O6 Cs1 O5 40.60(11) 3_645 8_655 ?
O3 Cs1 O5 107.14(12) . 8_655 ?
O9 Cs1 O5 108.24(12) 6_656 8_655 ?
O10 Cs1 O5 149.20(13) 6_656 8_655 ?
O13 Cs1 O5 85.24(13) 3_645 8_655 ?
Cs2 Cs1 O7 34.7(7) . 6_556 ?
O14 Cs1 O7 72.82(13) 2_554 6_556 ?
O1 Cs1 O7 85.36(12) . 6_556 ?
O6 Cs1 O7 120.35(13) 3_645 6_556 ?
O3 Cs1 O7 98.29(13) . 6_556 ?
O9 Cs1 O7 164.42(15) 6_656 6_556 ?
O10 Cs1 O7 125.92(12) 6_656 6_556 ?
O13 Cs1 O7 114.92(13) 3_645 6_556 ?
O5 Cs1 O7 84.79(12) 8_655 6_556 ?
Cs2 Cs1 O8 106.9(7) . 7_565 ?
O14 Cs1 O8 75.14(13) 2_554 7_565 ?
O1 Cs1 O8 70.23(11) . 7_565 ?
O6 Cs1 O8 156.90(15) 3_645 7_565 ?
O3 Cs1 O8 116.36(13) . 7_565 ?
O9 Cs1 O8 102.91(13) 6_656 7_565 ?
O10 Cs1 O8 65.19(11) 6_656 7_565 ?
O13 Cs1 O8 69.20(12) 3_645 7_565 ?
O5 Cs1 O8 132.88(13) 8_655 7_565 ?
O7 Cs1 O8 72.29(11) 6_556 7_565 ?
Cs2 Cs1 P1 81.2(7) . . ?
O14 Cs1 P1 157.76(13) 2_554 . ?
O1 Cs1 P1 23.35(8) . . ?
O6 Cs1 P1 106.86(11) 3_645 . ?
O3 Cs1 P1 24.35(8) . . ?
O9 Cs1 P1 79.49(11) 6_656 . ?
O10 Cs1 P1 65.06(10) 6_656 . ?
O13 Cs1 P1 144.56(13) 3_645 . ?
O5 Cs1 P1 126.83(10) 8_655 . ?
O7 Cs1 P1 85.86(10) 6_556 . ?
O8 Cs1 P1 92.66(10) 7_565 . ?
Cs1 Cs2 Cs3 35.1(13) . . ?
Cs1 Cs2 O14 85.3(7) . 2_554 ?
Cs3 Cs2 O14 75.6(13) . 2_554 ?
Cs1 Cs2 O1 76.3(7) . . ?
Cs3 Cs2 O1 68.4(13) . . ?
O14 Cs2 O1 139.2(2) 2_554 . ?
Cs1 Cs2 O3 90.2(7) . . ?
Cs3 Cs2 O3 104.7(13) . . ?
O14 Cs2 O3 171.3(2) 2_554 . ?
O1 Cs2 O3 45.93(12) . . ?
Cs1 Cs2 O6 81.9(7) . 3_645 ?
Cs3 Cs2 O6 115.1(12) . 3_645 ?
O14 Cs2 O6 89.24(17) 2_554 3_645 ?
O1 Cs2 O6 122.94(19) . 3_645 ?
O3 Cs2 O6 82.73(16) . 3_645 ?
Cs1 Cs2 O7 139.9(8) . 6_556 ?
Cs3 Cs2 O7 104.8(12) . 6_556 ?
O14 Cs2 O7 79.39(17) 2_554 6_556 ?
O1 Cs2 O7 91.57(17) . 6_556 ?
O3 Cs2 O7 108.68(17) . 6_556 ?
O6 Cs2 O7 134.14(18) 3_645 6_556 ?
Cs1 Cs2 O5 109.3(7) . 8_655 ?
Cs3 Cs2 O5 127.6(13) . 8_655 ?
O14 Cs2 O5 61.32(15) 2_554 8_655 ?
O1 Cs2 O5 159.5(2) . 8_655 ?
O3 Cs2 O5 113.58(18) . 8_655 ?
O6 Cs2 O5 42.14(12) 3_645 8_655 ?
O7 Cs2 O5 95.44(15) 6_556 8_655 ?
Cs1 Cs2 O12 105.4(8) . . ?
Cs3 Cs2 O12 135.3(12) . . ?
O14 Cs2 O12 135.2(2) 2_554 . ?
O1 Cs2 O12 85.23(15) . . ?
O3 Cs2 O12 39.40(12) . . ?
O6 Cs2 O12 51.13(13) 3_645 . ?
O7 Cs2 O12 111.59(16) 6_556 . ?
O5 Cs2 O12 74.24(14) 8_655 . ?
Cs1 Cs2 O3 177.2(8) . 6_556 ?
Cs3 Cs2 O3 144.1(12) . 6_556 ?
O14 Cs2 O3 96.97(16) 2_554 6_556 ?
O1 Cs2 O3 100.91(16) . 6_556 ?
O3 Cs2 O3 87.76(13) . 6_556 ?
O6 Cs2 O3 99.67(15) 3_645 6_556 ?
O7 Cs2 O3 39.63(11) 6_556 6_556 ?
O5 Cs2 O3 73.27(13) 8_655 6_556 ?
O12 Cs2 O3 74.06(13) . 6_556 ?
Cs1 Cs2 P1 90.5(7) . . ?
Cs3 Cs2 P1 91.1(13) . . ?
O14 Cs2 P1 162.3(2) 2_554 . ?
O1 Cs2 P1 24.00(9) . . ?
O3 Cs2 P1 24.66(9) . . ?
O6 Cs2 P1 107.18(16) 3_645 . ?
O7 Cs2 P1 93.11(14) 6_556 . ?
O5 Cs2 P1 135.91(17) 8_655 . ?
O12 Cs2 P1 62.44(11) . . ?
O3 Cs2 P1 86.89(12) 6_556 . ?
Cs1 Cs2 B2 103.4(7) . 8_655 ?
Cs3 Cs2 B2 133.2(13) . 8_655 ?
O14 Cs2 B2 82.12(18) 2_554 8_655 ?
O1 Cs2 B2 137.3(2) . 8_655 ?
O3 Cs2 B2 91.71(18) . 8_655 ?
O6 Cs2 B2 23.40(13) 3_645 8_655 ?
O7 Cs2 B2 110.77(17) 6_556 8_655 ?
O5 Cs2 B2 23.12(13) 8_655 8_655 ?
O12 Cs2 B2 53.16(15) . 8_655 ?
O3 Cs2 B2 78.47(15) 6_556 8_655 ?
P1 Cs2 B2 115.56(18) . 8_655 ?
Cs2 Cs3 O14 94.1(14) . 2_554 ?
Cs2 Cs3 O1 102.0(14) . . ?
O14 Cs3 O1 154.7(4) 2_554 . ?
Cs2 Cs3 O3 66.4(12) . . ?
O14 Cs3 O3 158.6(4) 2_554 . ?
O1 Cs3 O3 45.4(2) . . ?
Cs2 Cs3 O8 144.9(13) . 7_565 ?
O14 Cs3 O8 80.6(3) 2_554 7_565 ?
O1 Cs3 O8 74.9(2) . 7_565 ?
O3 Cs3 O8 120.3(3) . 7_565 ?
Cs2 Cs3 O7 66.3(12) . 6_556 ?
O14 Cs3 O7 77.7(3) 2_554 6_556 ?
O1 Cs3 O7 91.0(3) . 6_556 ?
O3 Cs3 O7 100.7(4) . 6_556 ?
O8 Cs3 O7 78.7(2) 7_565 6_556 ?
Cs2 Cs3 O10 136.9(14) . 6_656 ?
O14 Cs3 O10 124.9(4) 2_554 6_656 ?
O1 Cs3 O10 50.3(2) . 6_656 ?
O3 Cs3 O10 71.8(3) . 6_656 ?
O8 Cs3 O10 67.9(2) 7_565 6_656 ?
O7 Cs3 O10 133.4(3) 6_556 6_656 ?
Cs2 Cs3 O6 56.8(11) . 3_645 ?
O14 Cs3 O6 85.8(3) 2_554 3_645 ?
O1 Cs3 O6 119.4(3) . 3_645 ?
O3 Cs3 O6 76.4(2) . 3_645 ?
O8 Cs3 O6 154.8(4) 7_565 3_645 ?
O7 Cs3 O6 119.0(4) 6_556 3_645 ?
O10 Cs3 O6 104.1(3) 6_656 3_645 ?
Cs2 Cs3 O13 128.4(14) . 3_645 ?
O14 Cs3 O13 48.1(2) 2_554 3_645 ?
O1 Cs3 O13 126.9(4) . 3_645 ?
O3 Cs3 O13 138.3(4) . 3_645 ?
O8 Cs3 O13 72.1(3) 7_565 3_645 ?
O7 Cs3 O13 121.0(3) 6_556 3_645 ?
O10 Cs3 O13 78.9(3) 6_656 3_645 ?
O6 Cs3 O13 83.0(3) 3_645 3_645 ?
Cs2 Cs3 O9 109.5(12) . 6_656 ?
O14 Cs3 O9 116.4(4) 2_554 6_656 ?
O1 Cs3 O9 76.4(3) . 6_656 ?
O3 Cs3 O9 65.9(2) . 6_656 ?
O8 Cs3 O9 103.7(4) 7_565 6_656 ?
O7 Cs3 O9 165.9(4) 6_556 6_656 ?
O10 Cs3 O9 40.33(18) 6_656 6_656 ?
O6 Cs3 O9 63.8(2) 3_645 6_656 ?
O13 Cs3 O9 72.5(3) 3_645 6_656 ?
Cs2 Cs3 O5 45.6(12) . 8_655 ?
O14 Cs3 O5 57.5(2) 2_554 8_655 ?
O1 Cs3 O5 145.3(4) . 8_655 ?
O3 Cs3 O5 101.2(3) . 8_655 ?
O8 Cs3 O5 137.7(4) 7_565 8_655 ?
O7 Cs3 O5 86.2(3) 6_556 8_655 ?
O10 Cs3 O5 140.2(3) 6_656 8_655 ?
O6 Cs3 O5 38.25(14) 3_645 8_655 ?
O13 Cs3 O5 82.8(3) 3_645 8_655 ?
O9 Cs3 O5 100.4(2) 6_656 8_655 ?
Cs2 Cs3 O2 101.9(13) . 6_556 ?
O14 Cs3 O2 53.6(2) 2_554 6_556 ?
O1 Cs3 O2 103.4(3) . 6_556 ?
O3 Cs3 O2 136.1(4) . 6_556 ?
O8 Cs3 O2 47.57(16) 7_565 6_556 ?
O7 Cs3 O2 41.06(16) 6_556 6_556 ?
O10 Cs3 O2 115.4(3) 6_656 6_556 ?
O6 Cs3 O2 134.5(4) 3_645 6_556 ?
O13 Cs3 O2 83.2(3) 3_645 6_556 ?
O9 Cs3 O2 147.9(4) 6_656 6_556 ?
O5 Cs3 O2 97.0(3) 8_655 6_556 ?
O8 Ni1 O10 90.1(2) 6_656 6_656 ?
O8 Ni1 O1 174.74(19) 6_656 . ?
O10 Ni1 O1 85.90(18) 6_656 . ?
O8 Ni1 O2 90.23(18) 6_656 7_565 ?
O10 Ni1 O2 95.67(18) 6_656 7_565 ?
O1 Ni1 O2 93.58(17) . 7_565 ?
O8 Ni1 O11 97.45(19) 6_656 3_655 ?
O10 Ni1 O11 170.30(18) 6_656 3_655 ?
O1 Ni1 O11 86.88(17) . 3_655 ?
O2 Ni1 O11 78.32(17) 7_565 3_655 ?
O8 Ni1 O4 90.36(18) 6_656 6_656 ?
O10 Ni1 O4 86.26(18) 6_656 6_656 ?
O1 Ni1 O4 85.96(17) . 6_656 ?
O2 Ni1 O4 177.98(18) 7_565 6_656 ?
O11 Ni1 O4 99.69(17) 3_655 6_656 ?
O8 Ni1 Cs3 138.4(2) 6_656 . ?
O10 Ni1 Cs3 51.6(2) 6_656 . ?
O1 Ni1 Cs3 39.4(2) . . ?
O2 Ni1 Cs3 79.53(18) 7_565 . ?
O11 Ni1 Cs3 119.2(2) 3_655 . ?
O4 Ni1 Cs3 101.27(17) 6_656 . ?
O14 Ni2 O14 180.0 5_656 . ?
O14 Ni2 O11 92.87(18) 5_656 5_656 ?
O14 Ni2 O11 87.13(18) . 5_656 ?
O14 Ni2 O11 87.13(18) 5_656 . ?
O14 Ni2 O11 92.88(18) . . ?
O11 Ni2 O11 180.0 5_656 . ?
O14 Ni2 O2 86.48(19) 5_656 5_656 ?
O14 Ni2 O2 93.52(19) . 5_656 ?
O11 Ni2 O2 104.66(16) 5_656 5_656 ?
O11 Ni2 O2 75.34(16) . 5_656 ?
O14 Ni2 O2 93.52(19) 5_656 . ?
O14 Ni2 O2 86.48(19) . . ?
O11 Ni2 O2 75.34(16) 5_656 . ?
O11 Ni2 O2 104.66(16) . . ?
O2 Ni2 O2 180.0 5_656 . ?
O14 Ni2 Cs3 34.8(2) 5_656 6_656 ?
O14 Ni2 Cs3 145.2(2) . 6_656 ?
O11 Ni2 Cs3 83.5(2) 5_656 6_656 ?
O11 Ni2 Cs3 96.5(2) . 6_656 ?
O2 Ni2 Cs3 121.30(18) 5_656 6_656 ?
O2 Ni2 Cs3 58.70(18) . 6_656 ?
O14 Ni2 Cs3 145.2(2) 5_656 2 ?
O14 Ni2 Cs3 34.8(2) . 2 ?
O11 Ni2 Cs3 96.5(2) 5_656 2 ?
O11 Ni2 Cs3 83.5(2) . 2 ?
O2 Ni2 Cs3 58.70(18) 5_656 2 ?
O2 Ni2 Cs3 121.30(18) . 2 ?
Cs3 Ni2 Cs3 180.0 6_656 2 ?
O1 P1 O5 108.2(2) . . ?
O1 P1 O6 112.6(2) . . ?
O5 P1 O6 107.9(2) . . ?
O1 P1 O3 111.3(2) . . ?
O5 P1 O3 106.5(2) . . ?
O6 P1 O3 110.1(3) . . ?
O1 P1 Cs2 60.22(18) . . ?
O5 P1 Cs2 92.20(18) . . ?
O6 P1 Cs2 159.86(19) . . ?
O3 P1 Cs2 61.03(19) . . ?
O1 P1 Cs1 55.50(17) . . ?
O5 P1 Cs1 100.12(18) . . ?
O6 P1 Cs1 151.97(18) . . ?
O3 P1 Cs1 61.28(17) . . ?
Cs2 P1 Cs1 8.28(8) . . ?
O1 P1 Cs3 52.3(2) . . ?
O5 P1 Cs3 97.3(3) . . ?
O6 P1 Cs3 154.2(3) . . ?
O3 P1 Cs3 66.0(2) . . ?
Cs2 P1 Cs3 8.4(2) . . ?
Cs1 P1 Cs3 5.02(16) . . ?
O10 P2 O11 112.5(3) . . ?
O10 P2 O12 111.4(3) . . ?
O11 P2 O12 109.8(3) . . ?
O10 P2 O9 106.1(3) . . ?
O11 P2 O9 109.5(3) . . ?
O12 P2 O9 107.3(3) . . ?
O10 P2 Cs1 54.88(18) . 6_556 ?
O11 P2 Cs1 123.17(19) . 6_556 ?
O12 P2 Cs1 126.6(2) . 6_556 ?
O9 P2 Cs1 51.40(17) . 6_556 ?
O10 P2 Cs3 50.9(2) . 6_556 ?
O11 P2 Cs3 122.5(3) . 6_556 ?
O12 P2 Cs3 127.6(3) . 6_556 ?
O9 P2 Cs3 55.4(2) . 6_556 ?
Cs1 P2 Cs3 4.07(14) 6_556 6_556 ?
O8 P3 O2 112.8(3) . . ?
O8 P3 O7 113.8(3) . . ?
O2 P3 O7 110.1(3) . . ?
O8 P3 O13 109.9(3) . . ?
O2 P3 O13 109.1(3) . . ?
O7 P3 O13 100.5(3) . . ?
O8 P3 Cs3 157.4(3) . 6_656 ?
O2 P3 Cs3 63.9(3) . 6_656 ?
O7 P3 Cs3 53.1(2) . 6_656 ?
O13 P3 Cs3 91.6(3) . 6_656 ?
O8 P3 Cs2 151.7(2) . 6_656 ?
O2 P3 Cs2 69.30(19) . 6_656 ?
O7 P3 Cs2 45.83(18) . 6_656 ?
O13 P3 Cs2 94.8(2) . 6_656 ?
Cs3 P3 Cs2 7.55(18) 6_656 6_656 ?
O8 P3 Cs3 48.9(2) . 7_566 ?
O2 P3 Cs3 89.3(2) . 7_566 ?
O7 P3 Cs3 159.3(2) . 7_566 ?
O13 P3 Cs3 79.2(3) . 7_566 ?
Cs3 P3 Cs3 147.3(2) 6_656 7_566 ?
Cs2 P3 Cs3 154.71(17) 6_656 7_566 ?
B2 O5 P1 126.8(4) . . ?
B2 O5 Cs2 93.9(3) . 8_665 ?
P1 O5 Cs2 139.3(2) . 8_665 ?
B2 O5 Cs1 92.3(3) . 8_665 ?
P1 O5 Cs1 140.1(2) . 8_665 ?
Cs2 O5 Cs1 8.21(9) 8_665 8_665 ?
B2 O5 Cs3 96.5(4) . 8_665 ?
P1 O5 Cs3 136.3(3) . 8_665 ?
Cs2 O5 Cs3 6.7(2) 8_665 8_665 ?
Cs1 O5 Cs3 4.6(2) 8_665 8_665 ?
P1 O1 Ni1 125.8(3) . . ?
P1 O1 Cs3 104.8(3) . . ?
Ni1 O1 Cs3 115.3(3) . . ?
P1 O1 Cs1 101.1(2) . . ?
Ni1 O1 Cs1 115.16(18) . . ?
Cs3 O1 Cs1 5.9(2) . . ?
P1 O1 Cs2 95.8(2) . . ?
Ni1 O1 Cs2 124.38(19) . . ?
Cs3 O1 Cs2 9.6(3) . . ?
Cs1 O1 Cs2 9.59(10) . . ?
P3 O2 Ni1 123.4(3) . 7_566 ?
P3 O2 Ni2 133.9(3) . . ?
Ni1 O2 Ni2 99.96(18) 7_566 . ?
P3 O2 Cs3 94.4(3) . 6_656 ?
Ni1 O2 Cs3 102.2(3) 7_566 6_656 ?
Ni2 O2 Cs3 90.3(2) . 6_656 ?
B1 O3 P1 125.2(4) . . ?
B1 O3 Cs2 105.6(3) . . ?
P1 O3 Cs2 94.3(2) . . ?
B1 O3 Cs1 112.8(3) . . ?
P1 O3 Cs1 94.37(19) . . ?
Cs2 O3 Cs1 9.43(9) . . ?
B1 O3 Cs3 114.5(4) . . ?
P1 O3 Cs3 89.6(2) . . ?
Cs2 O3 Cs3 8.9(2) . . ?
Cs1 O3 Cs3 5.1(2) . . ?
B1 O3 Cs2 88.0(3) . 6_656 ?
P1 O3 Cs2 123.8(2) . 6_656 ?
Cs2 O3 Cs2 121.3(2) . 6_656 ?
Cs1 O3 Cs2 114.23(14) . 6_656 ?
Cs3 O3 Cs2 118.7(3) . 6_656 ?
B2 O4 B1 126.0(5) . . ?
B2 O4 Ni1 111.7(4) . 6_556 ?
B1 O4 Ni1 118.2(4) . 6_556 ?
B2 O6 P1 128.7(4) 6_656 . ?
B2 O6 Cs1 105.9(3) 6_656 3_655 ?
P1 O6 Cs1 125.3(2) . 3_655 ?
B2 O6 Cs2 97.1(3) 6_656 3_655 ?
P1 O6 Cs2 134.1(2) . 3_655 ?
Cs1 O6 Cs2 9.53(9) 3_655 3_655 ?
B2 O6 Cs3 103.7(4) 6_656 3_655 ?
P1 O6 Cs3 127.4(3) . 3_655 ?
Cs1 O6 Cs3 2.3(3) 3_655 3_655 ?
Cs2 O6 Cs3 8.1(2) 3_655 3_655 ?
B1 O7 P3 127.7(4) . . ?
B1 O7 Cs2 104.6(4) . 6_656 ?
P3 O7 Cs2 114.2(2) . 6_656 ?
B1 O7 Cs3 112.8(4) . 6_656 ?
P3 O7 Cs3 105.7(3) . 6_656 ?
Cs2 O7 Cs3 8.8(2) 6_656 6_656 ?
B1 O7 Cs1 109.5(4) . 6_656 ?
P3 O7 Cs1 108.9(2) . 6_656 ?
Cs2 O7 Cs1 5.38(10) 6_656 6_656 ?
Cs3 O7 Cs1 3.4(2) 6_656 6_656 ?
P3 O8 Ni1 131.7(3) . 6_556 ?
P3 O8 Cs3 111.8(3) . 7_566 ?
Ni1 O8 Cs3 116.1(3) 6_556 7_566 ?
P3 O8 Cs1 109.5(2) . 7_566 ?
Ni1 O8 Cs1 118.10(18) 6_556 7_566 ?
Cs3 O8 Cs1 3.0(3) 7_566 7_566 ?
B2 O9 P2 128.8(4) 8_655 . ?
B2 O9 Cs1 122.2(4) 8_655 6_556 ?
P2 O9 Cs1 107.5(2) . 6_556 ?
B2 O9 Cs3 125.6(4) 8_655 6_556 ?
P2 O9 Cs3 103.9(3) . 6_556 ?
Cs1 O9 Cs3 3.8(2) 6_556 6_556 ?
B2 O9 Cs2 120.4(4) 8_655 6_556 ?
P2 O9 Cs2 110.1(2) . 6_556 ?
Cs1 O9 Cs2 4.65(10) 6_556 6_556 ?
Cs3 O9 Cs2 7.8(2) 6_556 6_556 ?
P2 O10 Ni1 132.2(3) . 6_556 ?
P2 O10 Cs1 104.1(2) . 6_556 ?
Ni1 O10 Cs1 104.17(17) 6_556 6_556 ?
P2 O10 Cs3 109.4(3) . 6_556 ?
Ni1 O10 Cs3 100.8(3) 6_556 6_556 ?
Cs1 O10 Cs3 5.39(17) 6_556 6_556 ?
P2 O11 Ni2 132.9(3) . . ?
P2 O11 Ni1 122.3(3) . 3_645 ?
Ni2 O11 Ni1 104.16(18) . 3_645 ?
B1 O12 P2 133.4(4) . . ?
B1 O12 Cs2 89.9(4) . . ?
P2 O12 Cs2 111.0(3) . . ?
B1 O12 Cs1 90.8(4) . . ?
P2 O12 Cs1 115.5(2) . . ?
Cs2 O12 Cs1 7.82(8) . . ?
P3 O13 Cs1 122.1(2) . 3_655 ?
P3 O13 Cs3 127.2(3) . 3_655 ?
Cs1 O13 Cs3 5.30(17) 3_655 3_655 ?
P3 O13 H3 104(8) . . ?
Cs1 O13 H3 133(8) 3_655 . ?
Cs3 O13 H3 128(8) 3_655 . ?
Ni2 O14 Cs3 122.5(3) . 2 ?
Ni2 O14 Cs2 124.2(2) . 2 ?
Cs3 O14 Cs2 10.3(3) 2 2 ?
Ni2 O14 Cs1 128.5(2) . 2 ?
Cs3 O14 Cs1 6.0(2) 2 2 ?
Cs2 O14 Cs1 10.10(10) 2 2 ?
Ni2 O14 H1 118(5) . . ?
Cs3 O14 H1 79(5) 2 . ?
Cs2 O14 H1 87(5) 2 . ?
Cs1 O14 H1 77(5) 2 . ?
Ni2 O14 H2 114(9) . . ?
Cs3 O14 H2 116(9) 2 . ?
Cs2 O14 H2 108(8) 2 . ?
Cs1 O14 H2 110(9) 2 . ?
H1 O14 H2 101(9) . . ?
O4 B1 O12 111.3(5) . . ?
O4 B1 O7 112.8(5) . . ?
O12 B1 O7 108.8(5) . . ?
O4 B1 O3 111.7(5) . . ?
O12 B1 O3 105.1(5) . . ?
O7 B1 O3 106.8(5) . . ?
O4 B1 Cs2 164.7(4) . 6_656 ?
O12 B1 Cs2 82.2(3) . 6_656 ?
O7 B1 Cs2 54.1(3) . 6_656 ?
O3 B1 Cs2 69.5(3) . 6_656 ?
O4 B1 Cs2 91.3(4) . . ?
O12 B1 Cs2 68.1(4) . . ?
O7 B1 Cs2 154.1(4) . . ?
O3 B1 Cs2 52.8(3) . . ?
Cs2 B1 Cs2 100.57(19) 6_656 . ?
O4 B2 O5 114.7(5) . . ?
O4 B2 O9 110.6(5) . 8_665 ?
O5 B2 O9 104.9(5) . 8_665 ?
O4 B2 O6 110.9(5) . 6_556 ?
O5 B2 O6 105.9(5) . 6_556 ?
O9 B2 O6 109.5(5) 8_665 6_556 ?
O4 B2 Cs2 166.4(4) . 8_665 ?
O5 B2 Cs2 63.0(3) . 8_665 ?
O9 B2 Cs2 82.6(3) 8_665 8_665 ?
O6 B2 Cs2 59.5(3) 6_556 8_665 ?
O4 B2 Cs1 159.1(4) . 8_665 ?
O5 B2 Cs1 65.6(3) . 8_665 ?
O9 B2 Cs1 88.6(3) 8_665 8_665 ?
O6 B2 Cs1 52.5(3) 6_556 8_665 ?
Cs2 B2 Cs1 7.71(8) 8_665 8_665 ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O13 H3 O10  0.920(10) 1.550(13) 2.469(7) 178(12) 4_556
O14 H1 O13  0.917(10) 1.786(13) 2.702(7) 177(8) 4_456
O14 H2 O1  0.919(10) 1.83(5) 2.711(7) 159(12) 7_566
 
_refine_diff_density_max    0.983
_refine_diff_density_min   -0.981
_refine_diff_density_rms    0.189



