  
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         
;         
Dirubidium Diaquatrinickel-iron 24-oxodihydroxotetraborohexaphosphate(V)borophosphate
;
_chemical_name_common             'Rubidium nickel-iron borophosphate'
_chemical_melting_point           ?
_chemical_formula_moiety         'B8 Fe H12 Ni5 O56 P12,0.52(Rb2), 2.96(Rb)'
_chemical_formula_sum
 'B8 Fe H12 Ni5 O56 P12 Rb4' 
_chemical_formula_weight          2057.50

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'
 'Rb'  'Rb'  -0.9393   2.9676
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 '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                    9.4599(4)
_cell_length_b                    12.2035(4)
_cell_length_c                    19.9085(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2298.31(14)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2944
_cell_measurement_theta_min       2.912
_cell_measurement_theta_max       30.159
 
_exptl_crystal_description        'plateled column'
_exptl_crystal_colour             green
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.973          
_exptl_crystal_F_000              1988
_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     7.096
_shelx_estimated_absorpt_T_min    0.558
_shelx_estimated_absorpt_T_max    0.826
_exptl_absorpt_correction_type    'gaussian'
_exptl_absorpt_correction_T_min   0.399
_exptl_absorpt_correction_T_max   0.696
_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             15465
_diffrn_reflns_av_unetI/netI      0.0499
_diffrn_reflns_av_R_equivalents   0.0875
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.910
_diffrn_reflns_theta_max          24.976
_diffrn_reflns_theta_full         24.976
_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              2023
_reflns_number_gt                 1808
_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_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)+(0.0140P)²+14.0253P] 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      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2023
_refine_ls_number_parameters      196
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.0720
_refine_ls_R_factor_gt            0.0618
_refine_ls_wR_factor_ref          0.0972
_refine_ls_wR_factor_gt           0.0943
_refine_ls_goodness_of_fit_ref    1.315
_refine_ls_restrained_S_all       1.314
_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
Rb1 Rb 0.36831(19) 0.07736(14) 0.14735(9) 0.0460(4) Uani 0.74 1 d . . P . .
Rb2 Rb 0.2933(10) 0.1051(8) 0.1626(5) 0.0460(4) Uani 0.13 1 d . . P . .
Rb3 Rb 0.3371(12) 0.1071(9) 0.1243(6) 0.0460(4) Uani 0.13 1 d . . P . .
Ni1 Ni 0.68168(9) 0.30809(7) 0.08130(4) 0.0062(2) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.0000 0.5000 0.0091(3) Uani 0.5 2 d S . P . .
Fe2 Fe 0.5000 0.0000 0.5000 0.0091(3) Uani 0.5 2 d S . P . .
P1 P 0.50404(19) 0.33663(14) 0.21460(8) 0.0060(4) Uani 1 1 d . . . . .
P2 P 0.27314(18) 0.05923(15) 0.37811(8) 0.0065(4) Uani 1 1 d . . . . .
P3 P 0.5067(2) 0.27788(15) 0.45384(8) 0.0087(4) Uani 1 1 d . . . . .
O5 O 0.3694(5) 0.4040(4) 0.2280(2) 0.0077(10) Uani 1 1 d . . . . .
O1 O 0.5061(5) 0.3047(4) 0.1422(2) 0.0082(10) Uani 1 1 d . . . . .
O2 O 0.5636(5) 0.1790(4) 0.4924(2) 0.0122(11) Uani 1 1 d . . . . .
O3 O 0.4960(5) 0.2349(4) 0.2601(2) 0.0087(10) Uani 1 1 d . . . . .
O4 O 0.3006(5) 0.3006(4) 0.3279(2) 0.0071(10) Uani 1 1 d . . . . .
O6 O 0.6324(5) 0.4080(4) 0.2343(2) 0.0108(8) Uani 1 1 d . . . . .
O7 O 0.5307(5) 0.2651(4) 0.3770(2) 0.0133(11) Uani 1 1 d . . . . .
O8 O 0.3575(5) 0.3036(4) 0.4723(2) 0.0134(8) Uani 1 1 d . . . . .
O9 O 0.1805(5) -0.0033(4) 0.3276(2) 0.0100(10) Uani 1 1 d . . . . .
O10 O 0.1763(5) 0.1403(4) 0.4131(2) 0.0134(8) Uani 1 1 d . . . . .
O11 O 0.3436(5) -0.0213(4) 0.4262(2) 0.0091(10) Uani 1 1 d . . . . .
O12 O 0.3891(5) 0.1175(4) 0.3379(2) 0.0108(8) Uani 1 1 d . . . . .
O13 O 0.6026(6) 0.3806(4) 0.4684(2) 0.0161(12) Uani 1 1 d D . . . .
O14 O 0.3578(5) 0.0435(5) 0.5703(2) 0.0163(12) Uani 1 1 d D . . . .
B1 B 0.4247(8) 0.2316(7) 0.3274(4) 0.0069(12) Uani 1 1 d . . . . .
B2 B 0.2814(8) 0.3985(7) 0.2888(4) 0.0069(12) Uani 1 1 d . . . . .
H1 H 0.278(6) 0.073(8) 0.551(4) 0.06(3) Uiso 1 1 d D . . . .
H2 H 0.401(9) 0.096(6) 0.596(4) 0.05(3) Uiso 1 1 d D . . . .
H3 H 0.633(9) 0.386(7) 0.5121(15) 0.04(3) 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
Rb1 Rb3 0.656(10) . ?
Rb1 Rb2 0.843(10) . ?
Rb1 O14 3.018(5) 2_554 ?
Rb1 O1 3.067(5) . ?
Rb1 O6 3.134(5) 3_645 ?
Rb1 O9 3.152(5) 6_656 ?
Rb1 O3 3.193(5) . ?
Rb1 O10 3.244(5) 6_656 ?
Rb1 O13 3.339(5) 3_645 ?
Rb1 O5 3.480(5) 8_655 ?
Rb1 P1 3.668(2) . ?
Rb1 P2 3.869(3) 6_656 ?
Rb2 Rb3 0.868(14) . ?
Rb2 O14 2.951(10) 2_554 ?
Rb2 O3 3.156(10) . ?
Rb2 O5 3.176(10) 8_655 ?
Rb2 O1 3.186(10) . ?
Rb2 O6 3.240(11) 3_645 ?
Rb2 O7 3.256(11) 6_556 ?
Rb2 O3 3.576(11) 6_556 ?
Rb2 O12 3.610(10) . ?
Rb2 P1 3.611(9) . ?
Rb2 B2 3.630(12) 8_655 ?
Rb3 O14 2.817(12) 2_554 ?
Rb3 O1 2.915(12) . ?
Rb3 O8 3.222(12) 7_565 ?
Rb3 O10 3.319(13) 6_656 ?
Rb3 O13 3.372(13) 3_645 ?
Rb3 O3 3.465(12) . ?
Rb3 O7 3.481(12) 6_556 ?
Rb3 O2 3.587(11) 6_556 ?
Rb3 P1 3.685(11) . ?
Rb3 P3 4.007(12) 7_565 ?
Ni1 O8 1.977(5) 6_656 ?
Ni1 O10 2.052(5) 6_656 ?
Ni1 O1 2.057(4) . ?
Ni1 O2 2.098(5) 7_565 ?
Ni1 O11 2.101(5) 3_655 ?
Ni1 O4 2.131(4) 6_656 ?
Ni2 O14 2.012(5) . ?
Ni2 O14 2.012(5) 5_656 ?
Ni2 O11 2.101(4) 5_656 ?
Ni2 O11 2.101(4) . ?
Ni2 O2 2.271(5) . ?
Ni2 O2 2.271(5) 5_656 ?
Fe2 O14 2.012(5) . ?
Fe2 O14 2.012(5) 5_656 ?
Fe2 O11 2.101(4) 5_656 ?
Fe2 O11 2.101(4) . ?
Fe2 O2 2.271(5) . ?
Fe2 O2 2.271(5) 5_656 ?
P1 O1 1.493(4) . ?
P1 O3 1.539(5) . ?
P1 O5 1.539(5) . ?
P1 O6 1.544(5) . ?
P2 O10 1.517(5) . ?
P2 O11 1.526(5) . ?
P2 O12 1.533(5) . ?
P2 O9 1.537(5) . ?
P2 Rb1 3.869(3) 6_556 ?
P3 O8 1.491(5) . ?
P3 O2 1.528(5) . ?
P3 O7 1.554(4) . ?
P3 O13 1.574(5) . ?
P3 Rb3 4.007(12) 7_566 ?
P3 Rb3 4.066(11) 6_656 ?
O5 B2 1.471(8) . ?
O5 Rb2 3.176(10) 8_665 ?
O5 Rb1 3.480(5) 8_665 ?
O2 Ni1 2.098(5) 7_566 ?
O2 Rb3 3.587(11) 6_656 ?
O3 B1 1.501(8) . ?
O3 Rb2 3.576(11) 6_656 ?
O4 B2 1.437(9) . ?
O4 B1 1.445(9) . ?
O4 Ni1 2.131(4) 6_556 ?
O6 B2 1.488(9) 6_656 ?
O6 Rb1 3.134(5) 3_655 ?
O6 Rb2 3.240(11) 3_655 ?
O7 B1 1.465(9) . ?
O7 Rb2 3.256(11) 6_656 ?
O7 Rb3 3.481(12) 6_656 ?
O8 Ni1 1.977(5) 6_556 ?
O8 Rb3 3.222(12) 7_566 ?
O9 B2 1.471(9) 8_655 ?
O9 Rb1 3.152(5) 6_556 ?
O10 Ni1 2.052(5) 6_556 ?
O10 Rb1 3.244(5) 6_556 ?
O10 Rb3 3.319(13) 6_556 ?
O11 Ni1 2.101(5) 3_645 ?
O12 B1 1.448(9) . ?
O13 Rb1 3.339(5) 3_655 ?
O13 Rb3 3.371(13) 3_655 ?
O13 H3 0.917(10) . ?
O14 Rb3 2.817(12) 2 ?
O14 Rb2 2.951(10) 2 ?
O14 Rb1 3.018(5) 2 ?
O14 H1 0.918(10) . ?
O14 H2 0.919(11) . ?
B2 O9 1.471(9) 8_665 ?
B2 O6 1.488(9) 6_556 ?
B2 Rb2 3.630(12) 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
Rb3 Rb1 Rb2 69.5(11) . . ?
Rb3 Rb1 O14 66.1(10) . 2_554 ?
Rb2 Rb1 O14 77.4(6) . 2_554 ?
Rb3 Rb1 O1 70.6(10) . . ?
Rb2 Rb1 O1 90.4(7) . . ?
O14 Rb1 O1 136.59(14) 2_554 . ?
Rb3 Rb1 O6 153.0(11) . 3_645 ?
Rb2 Rb1 O6 89.6(7) . 3_645 ?
O14 Rb1 O6 93.34(14) 2_554 3_645 ?
O1 Rb1 O6 128.50(13) . 3_645 ?
Rb3 Rb1 O9 134.9(11) . 6_656 ?
Rb2 Rb1 O9 149.0(7) . 6_656 ?
O14 Rb1 O9 126.30(15) 2_554 6_656 ?
O1 Rb1 O9 83.67(13) . 6_656 ?
O6 Rb1 O9 71.15(12) 3_645 6_656 ?
Rb3 Rb1 O3 109.3(11) . . ?
Rb2 Rb1 O3 79.9(6) . . ?
O14 Rb1 O3 156.93(15) 2_554 . ?
O1 Rb1 O3 46.99(11) . . ?
O6 Rb1 O3 82.50(12) 3_645 . ?
O9 Rb1 O3 73.87(12) 6_656 . ?
Rb3 Rb1 O10 90.8(11) . 6_656 ?
Rb2 Rb1 O10 142.7(7) . 6_656 ?
O14 Rb1 O10 124.33(14) 2_554 6_656 ?
O1 Rb1 O10 52.55(12) . 6_656 ?
O6 Rb1 O10 115.88(13) 3_645 6_656 ?
O9 Rb1 O10 44.87(12) 6_656 6_656 ?
O3 Rb1 O10 77.19(12) . 6_656 ?
Rb3 Rb1 O13 87.2(11) . 3_645 ?
Rb2 Rb1 O13 127.3(6) . 3_645 ?
O14 Rb1 O13 49.92(14) 2_554 3_645 ?
O1 Rb1 O13 126.33(13) . 3_645 ?
O6 Rb1 O13 92.55(13) 3_645 3_645 ?
O9 Rb1 O13 78.90(13) 6_656 3_645 ?
O3 Rb1 O13 152.48(14) . 3_645 ?
O10 Rb1 O13 80.81(13) 6_656 3_645 ?
Rb3 Rb1 O5 111.6(11) . 8_655 ?
Rb2 Rb1 O5 62.2(7) . 8_655 ?
O14 Rb1 O5 58.62(12) 2_554 8_655 ?
O1 Rb1 O5 147.12(12) . 8_655 ?
O6 Rb1 O5 41.49(11) 3_645 8_655 ?
O9 Rb1 O5 110.03(12) 6_656 8_655 ?
O3 Rb1 O5 106.63(11) . 8_655 ?
O10 Rb1 O5 153.54(13) 6_656 8_655 ?
O13 Rb1 O5 86.25(12) 3_645 8_655 ?
Rb3 Rb1 P1 86.4(10) . . ?
Rb2 Rb1 P1 79.5(6) . . ?
O14 Rb1 P1 148.82(12) 2_554 . ?
O1 Rb1 P1 23.51(8) . . ?
O6 Rb1 P1 107.17(10) 3_645 . ?
O9 Rb1 P1 83.31(10) 6_656 . ?
O3 Rb1 P1 24.69(8) . . ?
O10 Rb1 P1 67.47(9) 6_656 . ?
O13 Rb1 P1 147.49(11) 3_645 . ?
O5 Rb1 P1 125.60(9) 8_655 . ?
Rb3 Rb1 P2 112.7(11) . 6_656 ?
Rb2 Rb1 P2 154.7(6) . 6_656 ?
O14 Rb1 P2 127.38(12) 2_554 6_656 ?
O1 Rb1 P2 68.09(10) . 6_656 ?
O6 Rb1 P2 93.60(10) 3_645 6_656 ?
O9 Rb1 P2 22.45(8) 6_656 6_656 ?
O3 Rb1 P2 75.64(9) . 6_656 ?
O10 Rb1 P2 22.50(9) 6_656 6_656 ?
O13 Rb1 P2 77.69(10) 3_645 6_656 ?
O5 Rb1 P2 131.70(9) 8_655 6_656 ?
P1 Rb1 P2 75.56(5) . 6_656 ?
Rb1 Rb2 Rb3 45.0(9) . . ?
Rb1 Rb2 O14 86.4(7) . 2_554 ?
Rb3 Rb2 O14 72.7(9) . 2_554 ?
Rb1 Rb2 O3 84.9(6) . . ?
Rb3 Rb2 O3 103.6(10) . . ?
O14 Rb2 O3 170.4(4) 2_554 . ?
Rb1 Rb2 O5 104.2(7) . 8_655 ?
Rb3 Rb2 O5 127.8(10) . 8_655 ?
O14 Rb2 O5 63.0(2) 2_554 8_655 ?
O3 Rb2 O5 115.5(3) . 8_655 ?
Rb1 Rb2 O1 74.3(6) . . ?
Rb3 Rb2 O1 64.2(9) . . ?
O14 Rb2 O1 134.2(4) 2_554 . ?
O3 Rb2 O1 46.40(16) . . ?
O5 Rb2 O1 161.6(4) 8_655 . ?
Rb1 Rb2 O6 75.3(7) . 3_645 ?
Rb3 Rb2 O6 118.3(11) . 3_645 ?
O14 Rb2 O6 92.5(3) 2_554 3_645 ?
O3 Rb2 O6 81.4(2) . 3_645 ?
O5 Rb2 O6 43.25(17) 8_655 3_645 ?
O1 Rb2 O6 120.7(3) . 3_645 ?
Rb1 Rb2 O7 142.8(9) . 6_556 ?
Rb3 Rb2 O7 97.7(11) . 6_556 ?
O14 Rb2 O7 81.3(3) 2_554 6_556 ?
O3 Rb2 O7 108.1(3) . 6_556 ?
O5 Rb2 O7 101.1(3) 8_655 6_556 ?
O1 Rb2 O7 89.6(3) . 6_556 ?
O6 Rb2 O7 139.8(4) 3_645 6_556 ?
Rb1 Rb2 O3 174.3(8) . 6_556 ?
Rb3 Rb2 O3 137.8(12) . 6_556 ?
O14 Rb2 O3 99.2(3) 2_554 6_556 ?
O3 Rb2 O3 89.5(2) . 6_556 ?
O5 Rb2 O3 77.6(2) 8_655 6_556 ?
O1 Rb2 O3 102.3(3) . 6_556 ?
O6 Rb2 O3 103.1(3) 3_645 6_556 ?
O7 Rb2 O3 40.42(16) 6_556 6_556 ?
Rb1 Rb2 O12 98.8(7) . . ?
Rb3 Rb2 O12 136.7(11) . . ?
O14 Rb2 O12 138.6(3) 2_554 . ?
O3 Rb2 O12 39.76(16) . . ?
O5 Rb2 O12 76.0(2) 8_655 . ?
O1 Rb2 O12 86.1(2) . . ?
O6 Rb2 O12 50.49(18) 3_645 . ?
O7 Rb2 O12 113.6(3) 6_556 . ?
O3 Rb2 O12 76.3(2) 6_556 . ?
Rb1 Rb2 P1 87.2(6) . . ?
Rb3 Rb2 P1 88.1(9) . . ?
O14 Rb2 P1 158.0(4) 2_554 . ?
O3 Rb2 P1 25.15(11) . . ?
O5 Rb2 P1 139.0(3) 8_655 . ?
O1 Rb2 P1 24.36(10) . . ?
O6 Rb2 P1 106.2(3) 3_645 . ?
O7 Rb2 P1 91.2(2) 6_556 . ?
O3 Rb2 P1 87.9(2) 6_556 . ?
O12 Rb2 P1 63.31(17) . . ?
Rb1 Rb2 B2 97.7(8) . 8_655 ?
Rb3 Rb2 B2 136.1(11) . 8_655 ?
O14 Rb2 B2 84.8(3) 2_554 8_655 ?
O3 Rb2 B2 92.3(3) . 8_655 ?
O5 Rb2 B2 23.78(15) 8_655 8_655 ?
O1 Rb2 B2 137.9(3) . 8_655 ?
O6 Rb2 B2 24.17(16) 3_645 8_655 ?
O7 Rb2 B2 115.8(3) 6_556 8_655 ?
O3 Rb2 B2 81.8(3) 6_556 8_655 ?
O12 Rb2 B2 53.7(2) . 8_655 ?
P1 Rb2 B2 116.9(3) . 8_655 ?
Rb1 Rb3 Rb2 65.4(11) . . ?
Rb1 Rb3 O14 101.6(11) . 2_554 ?
Rb2 Rb3 O14 90.2(10) . 2_554 ?
Rb1 Rb3 O1 97.2(11) . . ?
Rb2 Rb3 O1 100.2(10) . . ?
O14 Rb3 O1 161.0(4) 2_554 . ?
Rb1 Rb3 O8 144.9(13) . 7_565 ?
Rb2 Rb3 O8 149.7(12) . 7_565 ?
O14 Rb3 O8 84.4(3) 2_554 7_565 ?
O1 Rb3 O8 78.6(3) . 7_565 ?
Rb1 Rb3 O10 77.8(11) . 6_656 ?
Rb2 Rb3 O10 131.4(11) . 6_656 ?
O14 Rb3 O10 128.9(4) 2_554 6_656 ?
O1 Rb3 O10 52.9(2) . 6_656 ?
O8 Rb3 O10 72.0(3) 7_565 6_656 ?
Rb1 Rb3 O13 81.6(11) . 3_645 ?
Rb2 Rb3 O13 122.5(11) . 3_645 ?
O14 Rb3 O13 50.7(2) 2_554 3_645 ?
O1 Rb3 O13 130.7(4) . 3_645 ?
O8 Rb3 O13 75.7(3) 7_565 3_645 ?
O10 Rb3 O13 79.3(3) 6_656 3_645 ?
Rb1 Rb3 O3 60.4(10) . . ?
Rb2 Rb3 O3 62.3(9) . . ?
O14 Rb3 O3 151.1(4) 2_554 . ?
O1 Rb3 O3 45.09(19) . . ?
O8 Rb3 O3 123.7(3) 7_565 . ?
O10 Rb3 O3 72.6(2) 6_656 . ?
O13 Rb3 O3 136.3(4) 3_645 . ?
Rb1 Rb3 O7 133.3(13) . 6_556 ?
Rb2 Rb3 O7 68.0(11) . 6_556 ?
O14 Rb3 O7 79.3(3) 2_554 6_556 ?
O1 Rb3 O7 90.0(3) . 6_556 ?
O8 Rb3 O7 81.7(3) 7_565 6_556 ?
O10 Rb3 O7 137.4(3) 6_656 6_556 ?
O13 Rb3 O7 126.2(3) 3_645 6_556 ?
O3 Rb3 O7 96.8(3) . 6_556 ?
Rb1 Rb3 O2 156.1(12) . 6_556 ?
Rb2 Rb3 O2 103.4(11) . 6_556 ?
O14 Rb3 O2 56.0(2) 2_554 6_556 ?
O1 Rb3 O2 105.8(3) . 6_556 ?
O8 Rb3 O2 49.62(19) 7_565 6_556 ?
O10 Rb3 O2 121.5(3) 6_656 6_556 ?
O13 Rb3 O2 88.2(3) 3_645 6_556 ?
O3 Rb3 O2 135.1(4) . 6_556 ?
O7 Rb3 O2 42.18(16) 6_556 6_556 ?
Rb1 Rb3 P1 83.4(10) . . ?
Rb2 Rb3 P1 78.3(9) . . ?
O14 Rb3 P1 164.4(4) 2_554 . ?
O1 Rb3 P1 22.51(12) . . ?
O8 Rb3 P1 100.1(3) 7_565 . ?
O10 Rb3 P1 66.5(2) 6_656 . ?
O13 Rb3 P1 144.9(4) 3_645 . ?
O3 Rb3 P1 24.61(11) . . ?
O7 Rb3 P1 86.5(3) 6_556 . ?
O2 Rb3 P1 116.1(3) 6_556 . ?
Rb1 Rb3 P3 127.4(12) . 7_565 ?
Rb2 Rb3 P3 160.9(11) . 7_565 ?
O14 Rb3 P3 99.7(3) 2_554 7_565 ?
O1 Rb3 P3 66.1(2) . 7_565 ?
O8 Rb3 P3 20.32(12) 7_565 7_565 ?
O10 Rb3 P3 51.73(18) 6_656 7_565 ?
O13 Rb3 P3 75.9(3) 3_645 7_565 ?
O3 Rb3 P3 109.2(3) . 7_565 ?
O7 Rb3 P3 97.6(3) 6_556 7_565 ?
O2 Rb3 P3 69.8(2) 6_556 7_565 ?
P1 Rb3 P3 88.6(2) . 7_565 ?
O8 Ni1 O10 91.3(2) 6_656 6_656 ?
O8 Ni1 O1 175.59(19) 6_656 . ?
O10 Ni1 O1 85.85(19) 6_656 . ?
O8 Ni1 O2 89.72(18) 6_656 7_565 ?
O10 Ni1 O2 96.18(19) 6_656 7_565 ?
O1 Ni1 O2 93.93(17) . 7_565 ?
O8 Ni1 O11 94.9(2) 6_656 3_655 ?
O10 Ni1 O11 171.99(19) 6_656 3_655 ?
O1 Ni1 O11 88.29(18) . 3_655 ?
O2 Ni1 O11 78.76(18) 7_565 3_655 ?
O8 Ni1 O4 90.71(18) 6_656 6_656 ?
O10 Ni1 O4 85.63(18) 6_656 6_656 ?
O1 Ni1 O4 85.72(17) . 6_656 ?
O2 Ni1 O4 178.13(19) 7_565 6_656 ?
O11 Ni1 O4 99.39(17) 3_655 6_656 ?
O8 Ni1 Rb3 138.8(2) 6_656 . ?
O10 Ni1 Rb3 51.8(2) 6_656 . ?
O1 Ni1 Rb3 40.2(2) . . ?
O2 Ni1 Rb3 78.5(2) 7_565 . ?
O11 Ni1 Rb3 120.6(2) 3_655 . ?
O4 Ni1 Rb3 102.33(19) 6_656 . ?
O14 Ni2 O14 180.0 . 5_656 ?
O14 Ni2 O11 87.25(18) . 5_656 ?
O14 Ni2 O11 92.75(18) 5_656 5_656 ?
O14 Ni2 O11 92.75(18) . . ?
O14 Ni2 O11 87.25(18) 5_656 . ?
O11 Ni2 O11 180.0 5_656 . ?
O14 Ni2 O2 88.2(2) . . ?
O14 Ni2 O2 91.8(2) 5_656 . ?
O11 Ni2 O2 74.97(17) 5_656 . ?
O11 Ni2 O2 105.03(17) . . ?
O14 Ni2 O2 91.8(2) . 5_656 ?
O14 Ni2 O2 88.2(2) 5_656 5_656 ?
O11 Ni2 O2 105.03(17) 5_656 5_656 ?
O11 Ni2 O2 74.97(17) . 5_656 ?
O2 Ni2 O2 180.0 . 5_656 ?
O14 Fe2 O14 180.0 . 5_656 ?
O14 Fe2 O11 87.25(18) . 5_656 ?
O14 Fe2 O11 92.75(18) 5_656 5_656 ?
O14 Fe2 O11 92.75(18) . . ?
O14 Fe2 O11 87.25(18) 5_656 . ?
O11 Fe2 O11 180.0 5_656 . ?
O14 Fe2 O2 88.2(2) . . ?
O14 Fe2 O2 91.8(2) 5_656 . ?
O11 Fe2 O2 74.97(17) 5_656 . ?
O11 Fe2 O2 105.03(17) . . ?
O14 Fe2 O2 91.8(2) . 5_656 ?
O14 Fe2 O2 88.2(2) 5_656 5_656 ?
O11 Fe2 O2 105.03(17) 5_656 5_656 ?
O11 Fe2 O2 74.97(17) . 5_656 ?
O2 Fe2 O2 180.0 . 5_656 ?
O1 P1 O3 111.0(3) . . ?
O1 P1 O5 108.5(3) . . ?
O3 P1 O5 106.7(3) . . ?
O1 P1 O6 112.5(3) . . ?
O3 P1 O6 110.1(3) . . ?
O5 P1 O6 107.8(3) . . ?
O1 P1 Rb2 61.7(2) . . ?
O3 P1 Rb2 60.7(2) . . ?
O5 P1 Rb2 90.6(2) . . ?
O6 P1 Rb2 161.5(3) . . ?
O1 P1 Rb1 55.04(18) . . ?
O3 P1 Rb1 60.11(17) . . ?
O5 P1 Rb1 103.56(19) . . ?
O6 P1 Rb1 148.7(2) . . ?
Rb2 P1 Rb1 13.27(16) . . ?
O1 P1 Rb3 48.4(3) . . ?
O3 P1 Rb3 69.7(2) . . ?
O5 P1 Rb3 97.8(3) . . ?
O6 P1 Rb3 152.8(3) . . ?
Rb2 P1 Rb3 13.6(2) . . ?
Rb1 P1 Rb3 10.23(15) . . ?
O10 P2 O11 113.3(3) . . ?
O10 P2 O12 111.7(3) . . ?
O11 P2 O12 108.3(3) . . ?
O10 P2 O9 106.2(3) . . ?
O11 P2 O9 109.9(3) . . ?
O12 P2 O9 107.2(3) . . ?
O10 P2 Rb1 54.9(2) . 6_556 ?
O11 P2 Rb1 123.46(19) . 6_556 ?
O12 P2 Rb1 127.8(2) . 6_556 ?
O9 P2 Rb1 51.54(18) . 6_556 ?
O8 P3 O2 112.1(3) . . ?
O8 P3 O7 113.7(3) . . ?
O2 P3 O7 111.3(3) . . ?
O8 P3 O13 109.4(3) . . ?
O2 P3 O13 109.4(3) . . ?
O7 P3 O13 100.2(3) . . ?
O8 P3 Rb3 48.6(2) . 7_566 ?
O2 P3 Rb3 89.5(2) . 7_566 ?
O7 P3 Rb3 158.0(3) . 7_566 ?
O13 P3 Rb3 78.2(2) . 7_566 ?
O8 P3 Rb3 158.4(3) . 6_656 ?
O2 P3 Rb3 61.1(2) . 6_656 ?
O7 P3 Rb3 57.3(3) . 6_656 ?
O13 P3 Rb3 92.0(3) . 6_656 ?
Rb3 P3 Rb3 144.2(2) 7_566 6_656 ?
B2 O5 P1 125.9(4) . . ?
B2 O5 Rb2 95.7(4) . 8_665 ?
P1 O5 Rb2 137.9(3) . 8_665 ?
B2 O5 Rb1 92.4(4) . 8_665 ?
P1 O5 Rb1 141.2(2) . 8_665 ?
Rb2 O5 Rb1 13.57(18) 8_665 8_665 ?
P1 O1 Ni1 125.0(3) . . ?
P1 O1 Rb3 109.1(3) . . ?
Ni1 O1 Rb3 112.8(3) . . ?
P1 O1 Rb1 101.4(2) . . ?
Ni1 O1 Rb1 112.39(18) . . ?
Rb3 O1 Rb1 12.2(2) . . ?
P1 O1 Rb2 93.9(3) . . ?
Ni1 O1 Rb2 126.9(3) . . ?
Rb3 O1 Rb2 15.6(3) . . ?
Rb1 O1 Rb2 15.33(18) . . ?
P3 O2 Ni1 123.5(3) . 7_566 ?
P3 O2 Fe2 134.4(3) . . ?
Ni1 O2 Fe2 99.04(19) 7_566 . ?
P3 O2 Ni2 134.4(3) . . ?
Ni1 O2 Ni2 99.04(19) 7_566 . ?
Fe2 O2 Ni2 0.0 . . ?
P3 O2 Rb3 97.0(3) . 6_656 ?
Ni1 O2 Rb3 100.4(3) 7_566 6_656 ?
Fe2 O2 Rb3 89.9(2) . 6_656 ?
Ni2 O2 Rb3 89.9(2) . 6_656 ?
B1 O3 P1 124.7(4) . . ?
B1 O3 Rb2 105.2(4) . . ?
P1 O3 Rb2 94.2(3) . . ?
B1 O3 Rb1 116.2(4) . . ?
P1 O3 Rb1 95.19(19) . . ?
Rb2 O3 Rb1 15.24(18) . . ?
B1 O3 Rb3 119.3(4) . . ?
P1 O3 Rb3 85.7(2) . . ?
Rb2 O3 Rb3 14.1(2) . . ?
Rb1 O3 Rb3 10.29(17) . . ?
B1 O3 Rb2 87.5(4) . 6_656 ?
P1 O3 Rb2 124.9(3) . 6_656 ?
Rb2 O3 Rb2 121.4(3) . 6_656 ?
Rb1 O3 Rb2 109.5(2) . 6_656 ?
Rb3 O3 Rb2 118.5(2) . 6_656 ?
B2 O4 B1 125.7(5) . . ?
B2 O4 Ni1 110.9(4) . 6_556 ?
B1 O4 Ni1 117.4(4) . 6_556 ?
B2 O6 P1 128.5(4) 6_656 . ?
B2 O6 Rb1 106.6(4) 6_656 3_655 ?
P1 O6 Rb1 124.1(2) . 3_655 ?
B2 O6 Rb2 92.8(4) 6_656 3_655 ?
P1 O6 Rb2 138.6(3) . 3_655 ?
Rb1 O6 Rb2 15.07(18) 3_655 3_655 ?
B1 O7 P3 126.2(4) . . ?
B1 O7 Rb2 101.1(4) . 6_656 ?
P3 O7 Rb2 114.2(3) . 6_656 ?
B1 O7 Rb3 114.2(4) . 6_656 ?
P3 O7 Rb3 100.6(3) . 6_656 ?
Rb2 O7 Rb3 14.3(2) 6_656 6_656 ?
P3 O8 Ni1 132.0(3) . 6_556 ?
P3 O8 Rb3 111.1(3) . 7_566 ?
Ni1 O8 Rb3 116.5(3) 6_556 7_566 ?
B2 O9 P2 127.4(4) 8_655 . ?
B2 O9 Rb1 124.6(4) 8_655 6_556 ?
P2 O9 Rb1 106.0(2) . 6_556 ?
P2 O10 Ni1 131.4(3) . 6_556 ?
P2 O10 Rb1 102.6(2) . 6_556 ?
Ni1 O10 Rb1 106.19(19) 6_556 6_556 ?
P2 O10 Rb3 113.7(3) . 6_556 ?
Ni1 O10 Rb3 99.1(3) 6_556 6_556 ?
Rb1 O10 Rb3 11.39(17) 6_556 6_556 ?
P2 O11 Ni1 122.9(3) . 3_645 ?
P2 O11 Fe2 131.8(3) . . ?
Ni1 O11 Fe2 104.64(19) 3_645 . ?
P2 O11 Ni2 131.8(3) . . ?
Ni1 O11 Ni2 104.64(19) 3_645 . ?
Fe2 O11 Ni2 0.0 . . ?
B1 O12 P2 133.4(5) . . ?
B1 O12 Rb2 87.7(4) . . ?
P2 O12 Rb2 107.8(3) . . ?
P3 O13 Rb1 119.6(2) . 3_655 ?
P3 O13 Rb3 130.5(3) . 3_655 ?
Rb1 O13 Rb3 11.20(17) 3_655 3_655 ?
P3 O13 H3 114(6) . . ?
Rb1 O13 H3 125(6) 3_655 . ?
Rb3 O13 H3 114(6) 3_655 . ?
Fe2 O14 Ni2 0.0 . . ?
Fe2 O14 Rb3 122.0(3) . 2 ?
Ni2 O14 Rb3 122.0(3) . 2 ?
Fe2 O14 Rb2 126.5(3) . 2 ?
Ni2 O14 Rb2 126.5(3) . 2 ?
Rb3 O14 Rb2 17.1(3) 2 2 ?
Fe2 O14 Rb1 134.3(2) . 2 ?
Ni2 O14 Rb1 134.3(2) . 2 ?
Rb3 O14 Rb1 12.3(2) 2 2 ?
Rb2 O14 Rb1 16.18(19) 2 2 ?
Fe2 O14 H1 111(6) . . ?
Ni2 O14 H1 111(6) . . ?
Rb3 O14 H1 83(6) 2 . ?
Rb2 O14 H1 96(6) 2 . ?
Rb1 O14 H1 80(6) 2 . ?
Fe2 O14 H2 106(6) . . ?
Ni2 O14 H2 106(6) . . ?
Rb3 O14 H2 122(6) 2 . ?
Rb2 O14 H2 107(6) 2 . ?
Rb1 O14 H2 112(6) 2 . ?
H1 O14 H2 109(9) . . ?
O4 B1 O12 111.7(6) . . ?
O4 B1 O7 112.9(6) . . ?
O12 B1 O7 109.3(6) . . ?
O4 B1 O3 110.8(6) . . ?
O12 B1 O3 105.0(5) . . ?
O7 B1 O3 106.7(5) . . ?
O4 B2 O9 111.2(5) . 8_665 ?
O4 B2 O5 114.4(6) . . ?
O9 B2 O5 104.8(6) 8_665 . ?
O4 B2 O6 110.6(6) . 6_556 ?
O9 B2 O6 109.3(6) 8_665 6_556 ?
O5 B2 O6 106.1(5) . 6_556 ?
O4 B2 Rb2 167.7(5) . 8_665 ?
O9 B2 Rb2 81.1(4) 8_665 8_665 ?
O5 B2 Rb2 60.5(3) . 8_665 ?
O6 B2 Rb2 63.1(4) 6_556 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 
O14 H1 O13  0.918(10) 1.80(3) 2.698(7) 166(9) 4_456
O14 H2 O1  0.919(11) 1.815(17) 2.729(7) 173(9) 7_566
O13 H3 O10  0.917(10) 1.58(3) 2.474(6) 164(9) 4_556
 
_refine_diff_density_max    0.761
_refine_diff_density_min   -0.808
_refine_diff_density_rms    0.148



