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

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

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 1545738'
_audit_update_record             
;
2017-08-11 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(I4 Pb1.20), C14 H12 Co N2 O8'
_chemical_formula_sum            'C14 H12 Co I8 N2 O8 Pb2.40'
_chemical_formula_weight         1907.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   4.8667(3)
_cell_length_b                   11.3891(8)
_cell_length_c                   16.8685(12)
_cell_angle_alpha                82.028(6)
_cell_angle_beta                 89.129(6)
_cell_angle_gamma                83.994(5)
_cell_volume                     920.85(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    3091
_cell_measurement_theta_min      3.2100
_cell_measurement_theta_max      28.8160

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.440
_exptl_crystal_F_000             822
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    18.122
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.40139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11490
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.438
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_full        25.022
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3252
_reflns_number_gt                2536
_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 1.171.39.30c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2004)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_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)+(0.1044P)²+47.8146P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3252
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.2000
_refine_ls_wR_factor_gt          0.1848
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
I1 I -0.6663(3) 1.37700(11) 0.80588(8) 0.0299(4) Uani 1 1 d . . . . .
I2 I 0.2539(3) 0.67672(11) 0.95469(8) 0.0319(4) Uani 1 1 d . . . . .
I3 I -0.2718(4) 0.70321(13) 0.71610(11) 0.0506(5) Uani 1 1 d . . . . .
I4 I -0.1863(4) 1.36209(14) 0.58566(15) 0.0692(7) Uani 1 1 d . . . . .
Pb1 Pb -0.21864(18) 0.52705(8) 0.87652(5) 0.0187(4) Uani 0.727(4) 1 d . . . . .
Pb2 Pb 0.2699(3) 0.5410(2) 0.62843(12) 0.0481(9) Uani 0.475(4) 1 d . . . . .
Co1 Co 0.0000 1.0000 0.5000 0.0286(9) Uani 1 2 d S . P . .
O1 O -0.262(2) 1.0329(10) 0.5954(6) 0.017(2) Uani 1 1 d . . . . .
O2 O 0.056(2) 0.9831(12) 0.6933(7) 0.026(3) Uani 1 1 d . . . . .
O3 O -0.259(2) 0.8743(10) 0.4770(6) 0.014(2) Uani 1 1 d . . . . .
O4 O 0.241(2) 0.8630(12) 0.5714(7) 0.026(3) Uani 1 1 d . . . . .
N1 N -0.288(3) 1.0540(12) 0.8065(8) 0.018(3) Uani 1 1 d . . . . .
C1 C -0.174(3) 1.0244(14) 0.6677(10) 0.017(4) Uani 1 1 d . . . . .
C2 C -0.391(4) 1.0705(15) 0.7235(10) 0.020(4) Uani 1 1 d . . . . .
H2A H -0.4455 1.1563 0.7058 0.024 Uiso 1 1 calc R U . . .
H2B H -0.5573 1.0276 0.7213 0.024 Uiso 1 1 calc R U . . .
C3 C -0.354(3) 0.9615(16) 0.8577(10) 0.021(4) Uani 1 1 d . . . . .
H3 H -0.4799 0.9111 0.8416 0.025 Uiso 1 1 calc R U . . .
C4 C -0.242(3) 0.9370(16) 0.9340(11) 0.020(4) Uani 1 1 d . . . . .
H4 H -0.2913 0.8698 0.9692 0.024 Uiso 1 1 calc R U . . .
C5 C -0.061(3) 1.0097(14) 0.9595(10) 0.014(3) Uiso 1 1 d . . . . .
C6 C 0.006(4) 1.1082(15) 0.9039(10) 0.021(4) Uiso 1 1 d . . . . .
H6 H 0.1290 1.1608 0.9187 0.025 Uiso 1 1 calc R U . . .
C7 C -0.111(4) 1.1275(16) 0.8274(11) 0.021(4) Uiso 1 1 d . . . . .
H7 H -0.0644 1.1928 0.7900 0.025 Uiso 1 1 calc R U . . .


_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
I1 Pb1 3.2421(15) 1_565 ?
I1 Pb2 3.301(3) 1_465 ?
I1 Pb1 3.3274(16) 1_465 ?
I2 Pb1 3.2921(15) 1_655 ?
I2 Pb1 3.3867(16) . ?
I2 Pb1 3.4290(16) 2_567 ?
I3 Pb1 3.1341(18) . ?
I4 Pb2 3.301(2) 1_465 ?
I4 Pb2 3.317(3) 1_565 ?
Pb1 I1 3.2420(15) 1_545 ?
Pb1 I2 3.2921(15) 1_455 ?
Pb1 I1 3.3274(16) 1_645 ?
Pb1 I2 3.4290(16) 2_567 ?
Pb2 I4 3.301(2) 1_645 ?
Pb2 I1 3.301(3) 1_645 ?
Pb2 I4 3.317(3) 1_545 ?
Co1 O3 2.083(11) . ?
Co1 O3 2.083(11) 2_576 ?
Co1 O1 2.089(10) . ?
Co1 O1 2.089(10) 2_576 ?
Co1 O4 2.097(13) . ?
Co1 O4 2.097(13) 2_576 ?
O1 C1 1.29(2) . ?
O2 C1 1.23(2) . ?
N1 C3 1.33(2) . ?
N1 C7 1.35(2) . ?
N1 C2 1.48(2) . ?
C1 C2 1.51(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.39(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.42(2) . ?
C5 C5 1.48(3) 2_577 ?
C6 C7 1.40(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?

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
Pb1 I1 Pb2 96.37(5) 1_565 1_465 ?
Pb1 I1 Pb1 95.59(4) 1_565 1_465 ?
Pb2 I1 Pb1 92.12(5) 1_465 1_465 ?
Pb1 I2 Pb1 93.54(4) 1_655 . ?
Pb1 I2 Pb1 94.91(4) 1_655 2_567 ?
Pb1 I2 Pb1 85.84(4) . 2_567 ?
Pb2 I4 Pb2 94.68(7) 1_465 1_565 ?
I3 Pb1 I1 88.01(4) . 1_545 ?
I3 Pb1 I2 91.34(5) . 1_455 ?
I1 Pb1 I2 86.85(4) 1_545 1_455 ?
I3 Pb1 I1 90.47(5) . 1_645 ?
I1 Pb1 I1 95.59(4) 1_545 1_645 ?
I2 Pb1 I1 177.02(4) 1_455 1_645 ?
I3 Pb1 I2 93.67(5) . . ?
I1 Pb1 I2 178.27(4) 1_545 . ?
I2 Pb1 I2 93.54(4) 1_455 . ?
I1 Pb1 I2 83.97(4) 1_645 . ?
I3 Pb1 I2 171.58(5) . 2_567 ?
I1 Pb1 I2 84.19(4) 1_545 2_567 ?
I2 Pb1 I2 85.09(4) 1_455 2_567 ?
I1 Pb1 I2 93.43(4) 1_645 2_567 ?
I2 Pb1 I2 94.16(4) . 2_567 ?
I4 Pb2 I1 82.94(7) 1_645 1_645 ?
I4 Pb2 I4 94.68(6) 1_645 1_545 ?
I1 Pb2 I4 87.07(7) 1_645 1_545 ?
O3 Co1 O3 180.0(4) . 2_576 ?
O3 Co1 O1 87.0(4) . . ?
O3 Co1 O1 93.0(4) 2_576 . ?
O3 Co1 O1 93.0(4) . 2_576 ?
O3 Co1 O1 87.0(4) 2_576 2_576 ?
O1 Co1 O1 180.0(6) . 2_576 ?
O3 Co1 O4 88.3(5) . . ?
O3 Co1 O4 91.7(5) 2_576 . ?
O1 Co1 O4 92.2(4) . . ?
O1 Co1 O4 87.8(4) 2_576 . ?
O3 Co1 O4 91.7(5) . 2_576 ?
O3 Co1 O4 88.3(5) 2_576 2_576 ?
O1 Co1 O4 87.8(4) . 2_576 ?
O1 Co1 O4 92.2(4) 2_576 2_576 ?
O4 Co1 O4 180.0 . 2_576 ?
C1 O1 Co1 122.4(10) . . ?
C3 N1 C7 120.9(15) . . ?
C3 N1 C2 119.6(14) . . ?
C7 N1 C2 119.3(14) . . ?
O2 C1 O1 127.3(15) . . ?
O2 C1 C2 120.2(15) . . ?
O1 C1 C2 112.4(14) . . ?
N1 C2 C1 111.0(14) . . ?
N1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 121.4(16) . . ?
N1 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 120.6(17) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 117.0(16) . . ?
C4 C5 C5 123.3(19) . 2_577 ?
C6 C5 C5 119.7(18) . 2_577 ?
C7 C6 C5 119.8(16) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N1 C7 C6 120.3(16) . . ?
N1 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?

_refine_diff_density_max         6.203
_refine_diff_density_min         -6.457
_refine_diff_density_rms         0.366

####################################################################### 
# 
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1545737'
_audit_update_record             
;
2017-08-11 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C28 H24 I15 K3 N4 Ni O14.60 Pb4.50), 2(O) 18(H2 O)'
_chemical_formula_sum            'C56 H84 I30 K6 N8 Ni2 O49.20 Pb9'
_chemical_formula_weight         7355.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   23.839(5)
_cell_length_b                   23.108(5)
_cell_length_c                   15.993(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.99(3)
_cell_angle_gamma                90
_cell_volume                     8676(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    8257
_cell_measurement_theta_min      2.6010
_cell_measurement_theta_max      27.6750

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.816
_exptl_crystal_F_000             6375
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    14.437
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.20570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33116
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.186
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7867
_reflns_number_gt                5884
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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.

SQUEEZE removed 9 disordered H2O molecules per unit cell. 
This value calculated based upon TG analysis.
;

_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2004)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_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)+(0.0479P)²+186.8681P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7867
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Ni1 Ni 0.31151(8) 0.0000 -0.21808(11) 0.0227(4) Uani 1 2 d S T P . .
Pb1 Pb 0.5000 0.0000 0.5000 0.0306(2) Uani 1 4 d S T P . .
Pb2 Pb 0.36944(3) 0.0000 0.29920(4) 0.03045(16) Uani 1 2 d S T P . .
Pb3 Pb 0.20344(2) 0.11198(2) 0.20562(3) 0.03204(13) Uani 1 1 d . . . . .
Pb4 Pb 0.04133(3) 0.0000 0.13233(4) 0.03304(17) Uani 1 2 d S T P . .
I1 I 0.50917(5) 0.0000 0.30288(7) 0.0433(3) Uani 1 2 d S T P . .
I2 I 0.40090(3) 0.09514(3) 0.44975(5) 0.03398(19) Uani 1 1 d . . . . .
I3 I 0.24192(4) 0.0000 0.33524(6) 0.0307(2) Uani 1 2 d S T P . .
I4 I 0.33796(4) 0.09961(3) 0.16488(5) 0.0420(2) Uani 1 1 d . . . . .
I5 I 0.17197(5) 0.0000 0.06531(7) 0.0366(3) Uani 1 2 d S T P . .
I6 I 0.23749(5) 0.19856(4) 0.35108(6) 0.0534(3) Uani 1 1 d . . . . .
I7 I 0.16769(4) 0.21481(4) 0.08485(5) 0.0379(2) Uani 1 1 d . . . . .
I8 I 0.08496(4) 0.09801(4) 0.27133(5) 0.0416(2) Uani 1 1 d . . . . .
I9 I -0.07464(5) 0.0000 0.20156(8) 0.0440(3) Uani 1 2 d S T P . .
I10 I 0.0000 -0.09915(5) 0.0000 0.0359(3) Uani 1 2 d S T P . .
N1 N 0.1773(4) 0.1684(4) -0.1259(6) 0.033(2) Uani 1 1 d . . . . .
N2 N -0.0725(4) 0.3122(4) -0.3040(6) 0.034(2) Uani 1 1 d . . . . .
C1 C 0.2425(5) 0.0942(5) -0.1625(7) 0.030(3) Uani 1 1 d . . . . .
C2 C 0.2284(5) 0.1354(5) -0.0942(7) 0.032(3) Uani 1 1 d . . . . .
H2A H 0.2227 0.1130 -0.0436 0.038 Uiso 1 1 calc R U . . .
H2B H 0.2607 0.1623 -0.0768 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1809(6) 0.2164(5) -0.1683(9) 0.044(3) Uani 1 1 d . . . . .
H3 H 0.2172 0.2317 -0.1731 0.053 Uiso 1 1 calc R U . . .
C4 C 0.1318(5) 0.2450(5) -0.2065(8) 0.036(3) Uani 1 1 d . . . . .
H4 H 0.1349 0.2804 -0.2355 0.043 Uiso 1 1 calc R U . . .
C5 C 0.0785(5) 0.2227(5) -0.2028(7) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.0759(5) 0.1710(5) -0.1592(7) 0.031(3) Uani 1 1 d . . . . .
H6 H 0.0401 0.1544 -0.1548 0.038 Uiso 1 1 calc R U . . .
C7 C 0.1249(5) 0.1444(5) -0.1228(7) 0.036(3) Uani 1 1 d . . . . .
H7 H 0.1229 0.1085 -0.0946 0.043 Uiso 1 1 calc R U . . .
C8 C 0.0258(5) 0.2530(5) -0.2412(7) 0.033(3) Uani 1 1 d . . . . .
C9 C 0.0249(5) 0.2939(5) -0.3021(8) 0.041(3) Uani 1 1 d . . . . .
H9 H 0.0585 0.3018 -0.3244 0.049 Uiso 1 1 calc R U . . .
C10 C -0.0232(5) 0.3235(6) -0.3313(8) 0.041(3) Uani 1 1 d . . . . .
H10 H -0.0224 0.3531 -0.3722 0.049 Uiso 1 1 calc R U . . .
C11 C -0.0744(5) 0.2718(5) -0.2435(8) 0.038(3) Uani 1 1 d . . . . .
H11 H -0.1089 0.2648 -0.2232 0.046 Uiso 1 1 calc R U . . .
C12 C -0.0275(5) 0.2416(5) -0.2121(8) 0.034(3) Uani 1 1 d . . . . .
H12 H -0.0292 0.2126 -0.1706 0.041 Uiso 1 1 calc R U . . .
C13 C -0.1244(5) 0.3496(5) -0.3302(7) 0.037(3) Uani 1 1 d . . . . .
H13A H -0.1593 0.3258 -0.3335 0.045 Uiso 1 1 calc R U . . .
H13B H -0.1239 0.3662 -0.3871 0.045 Uiso 1 1 calc R U . . .
C14 C -0.1255(5) 0.3984(5) -0.2662(7) 0.030(3) Uani 1 1 d . . . . .
O1 O 0.2833(3) 0.0598(3) -0.1387(4) 0.0279(17) Uani 1 1 d . . . . .
O2 O 0.2135(3) 0.0981(4) -0.2339(5) 0.039(2) Uani 1 1 d . . . . .
O3 O -0.0940(4) 0.3954(4) -0.1963(5) 0.040(2) Uani 1 1 d . . . . .
O4 O -0.1618(3) 0.4369(3) -0.2929(4) 0.0263(17) Uani 1 1 d . . . . .
O5 O -0.2755(4) 0.5858(4) -0.4877(6) 0.056(3) Uani 1 1 d . . . . .
O6 O 0.3888(4) 0.0000 -0.1361(6) 0.030(3) Uani 1 2 d S T P . .
O7 O 0.2360(4) 0.0000 -0.3082(6) 0.023(2) Uani 1 2 d S T P . .
O8 O 0.0234(9) 0.0000 0.4177(10) 0.089(7) Uani 0.8 2 d S T P . .
O9 O 0.4516(9) 0.0000 0.0663(13) 0.145(14) Uani 0.8 2 d S T P . .
O10 O 0.0859(11) 0.0767(8) 0.6023(12) 0.075(7) Uani 0.5 1 d . . P . .
O11 O -0.1021(12) 0.3752(12) -0.0288(12) 0.102(10) Uani 0.5 1 d . . P . .
K1 K 0.3342(2) 0.0000 0.0013(2) 0.0582(13) Uani 1 2 d S T P . .
K2 K -0.19468(16) 0.5000 -0.4372(2) 0.0346(9) Uani 1 2 d S T P . .
K3 K 0.1360(3) 0.0000 0.4936(5) 0.093(2) Uani 1 2 d S T P . .


_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
Ni1 O4 2.055(7) 3_545 ?
Ni1 O4 2.055(7) 8 ?
Ni1 O1 2.066(7) . ?
Ni1 O1 2.067(7) 6 ?
Ni1 O6 2.067(10) . ?
Ni1 O7 2.101(9) . ?
Ni1 K1 3.455(4) . ?
Ni1 K2 3.481(4) 3_545 ?
Pb1 I1 3.1977(13) 5_656 ?
Pb1 I1 3.1978(13) . ?
Pb1 I2 3.2250(10) 6 ?
Pb1 I2 3.2250(9) 2_656 ?
Pb1 I2 3.2250(9) 5_656 ?
Pb1 I2 3.2250(9) . ?
Pb2 I4 3.1490(10) 6 ?
Pb2 I4 3.1491(10) . ?
Pb2 I3 3.1908(14) . ?
Pb2 I2 3.2505(10) . ?
Pb2 I2 3.2505(10) 6 ?
Pb2 I1 3.3213(15) . ?
Pb3 I6 3.0688(11) . ?
Pb3 I7 3.0874(10) . ?
Pb3 I8 3.1962(12) . ?
Pb3 I3 3.3429(9) . ?
Pb3 I4 3.3934(12) . ?
Pb3 I5 3.4220(10) . ?
Pb4 I9 3.1513(15) . ?
Pb4 I10 3.1584(10) 5 ?
Pb4 I10 3.1584(10) . ?
Pb4 I8 3.2172(11) 6 ?
Pb4 I8 3.2172(11) . ?
I2 K2 3.837(3) 3_546 ?
I3 Pb3 3.3429(9) 6 ?
I3 K2 3.691(4) 3_546 ?
I3 K3 3.874(6) . ?
I4 K1 3.475(3) . ?
I5 Pb3 3.4221(10) 6 ?
I10 Pb4 3.1584(10) 5 ?
N1 C3 1.311(15) . ?
N1 C7 1.375(15) . ?
N1 C2 1.453(14) . ?
N2 C10 1.348(15) . ?
N2 C11 1.351(14) . ?
N2 C13 1.508(14) . ?
C1 O2 1.231(13) . ?
C1 O1 1.262(13) . ?
C1 C2 1.531(15) . ?
C3 C4 1.390(17) . ?
C4 C5 1.382(16) . ?
C5 C6 1.390(16) . ?
C5 C8 1.475(17) . ?
C6 C7 1.358(16) . ?
C8 C9 1.355(16) . ?
C8 C12 1.452(17) . ?
C9 C10 1.347(17) . ?
C11 C12 1.339(16) . ?
C13 C14 1.525(16) . ?
C14 O3 1.235(14) . ?
C14 O4 1.263(13) . ?
O1 K1 2.730(8) . ?
O4 Ni1 2.055(7) 3_455 ?
O4 K2 2.727(7) . ?
O5 K2 2.785(9) . ?
O5 K3 2.872(11) 3_454 ?
O6 K1 2.741(11) . ?
O7 K2 2.857(10) 3_545 ?
O8 K3 2.75(2) . ?
O9 K1 2.81(2) . ?
O10 K3 2.883(19) . ?
O11 K1 3.33(3) 3_455 ?
K1 O1 2.730(8) 6 ?
K1 O11 3.33(3) 8 ?
K1 O11 3.33(3) 3_545 ?
K1 I4 3.475(3) 6 ?
K2 O4 2.727(7) 6_565 ?
K2 O5 2.785(9) 6_565 ?
K2 O7 2.857(10) 3_455 ?
K2 Ni1 3.481(4) 3_455 ?
K2 I3 3.691(4) 3_454 ?
K2 I2 3.837(3) 3_454 ?
K2 I2 3.837(3) 8_454 ?
K2 K3 3.996(7) 3_454 ?
K3 O5 2.872(11) 3_546 ?
K3 O5 2.872(11) 8_556 ?
K3 O10 2.883(19) 6 ?
K3 K2 3.996(7) 3_546 ?

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 Ni1 O4 90.3(4) 3_545 8 ?
O4 Ni1 O1 176.9(3) 3_545 . ?
O4 Ni1 O1 92.8(3) 8 . ?
O4 Ni1 O1 92.8(3) 3_545 6 ?
O4 Ni1 O1 176.9(3) 8 6 ?
O1 Ni1 O1 84.0(4) . 6 ?
O4 Ni1 O6 92.1(3) 3_545 . ?
O4 Ni1 O6 92.1(3) 8 . ?
O1 Ni1 O6 87.7(3) . . ?
O1 Ni1 O6 87.7(3) 6 . ?
O4 Ni1 O7 85.2(3) 3_545 . ?
O4 Ni1 O7 85.2(3) 8 . ?
O1 Ni1 O7 95.2(3) . . ?
O1 Ni1 O7 95.2(3) 6 . ?
O6 Ni1 O7 176.1(4) . . ?
O4 Ni1 K1 125.5(2) 3_545 . ?
O4 Ni1 K1 125.5(2) 8 . ?
O1 Ni1 K1 52.2(2) . . ?
O1 Ni1 K1 52.2(2) 6 . ?
O6 Ni1 K1 52.5(3) . . ?
O7 Ni1 K1 131.4(3) . . ?
O4 Ni1 K2 51.5(2) 3_545 3_545 ?
O4 Ni1 K2 51.5(2) 8 3_545 ?
O1 Ni1 K2 131.0(2) . 3_545 ?
O1 Ni1 K2 131.0(2) 6 3_545 ?
O6 Ni1 K2 121.0(3) . 3_545 ?
O7 Ni1 K2 55.1(3) . 3_545 ?
K1 Ni1 K2 173.51(12) . 3_545 ?
I1 Pb1 I1 180.0 5_656 . ?
I1 Pb1 I2 94.20(3) 5_656 6 ?
I1 Pb1 I2 85.80(3) . 6 ?
I1 Pb1 I2 85.80(3) 5_656 2_656 ?
I1 Pb1 I2 94.20(3) . 2_656 ?
I2 Pb1 I2 180.00(4) 6 2_656 ?
I1 Pb1 I2 85.80(3) 5_656 5_656 ?
I1 Pb1 I2 94.20(3) . 5_656 ?
I2 Pb1 I2 94.05(3) 6 5_656 ?
I2 Pb1 I2 85.95(3) 2_656 5_656 ?
I1 Pb1 I2 94.20(3) 5_656 . ?
I1 Pb1 I2 85.80(3) . . ?
I2 Pb1 I2 85.95(3) 6 . ?
I2 Pb1 I2 94.05(3) 2_656 . ?
I2 Pb1 I2 180.0 5_656 . ?
I4 Pb2 I4 93.93(4) 6 . ?
I4 Pb2 I3 90.08(3) 6 . ?
I4 Pb2 I3 90.08(3) . . ?
I4 Pb2 I2 175.33(3) 6 . ?
I4 Pb2 I2 90.46(3) . . ?
I3 Pb2 I2 88.32(3) . . ?
I4 Pb2 I2 90.46(3) 6 6 ?
I4 Pb2 I2 175.34(3) . 6 ?
I3 Pb2 I2 88.32(3) . 6 ?
I2 Pb2 I2 85.12(4) . 6 ?
I4 Pb2 I1 97.56(3) 6 . ?
I4 Pb2 I1 97.56(3) . . ?
I3 Pb2 I1 168.76(3) . . ?
I2 Pb2 I1 83.41(3) . . ?
I2 Pb2 I1 83.41(3) 6 . ?
I6 Pb3 I7 88.88(3) . . ?
I6 Pb3 I8 87.09(3) . . ?
I7 Pb3 I8 96.87(3) . . ?
I6 Pb3 I3 91.52(3) . . ?
I7 Pb3 I3 179.60(3) . . ?
I8 Pb3 I3 83.17(3) . . ?
I6 Pb3 I4 93.79(3) . . ?
I7 Pb3 I4 96.44(3) . . ?
I8 Pb3 I4 166.67(3) . . ?
I3 Pb3 I4 83.51(3) . . ?
I6 Pb3 I5 171.54(3) . . ?
I7 Pb3 I5 99.58(3) . . ?
I8 Pb3 I5 91.92(3) . . ?
I3 Pb3 I5 80.02(3) . . ?
I4 Pb3 I5 85.26(3) . . ?
I9 Pb4 I10 92.57(3) . 5 ?
I9 Pb4 I10 92.57(3) . . ?
I10 Pb4 I10 93.01(4) 5 . ?
I9 Pb4 I8 87.44(3) . 6 ?
I10 Pb4 I8 178.24(3) 5 6 ?
I10 Pb4 I8 88.75(3) . 6 ?
I9 Pb4 I8 87.44(3) . . ?
I10 Pb4 I8 88.75(3) 5 . ?
I10 Pb4 I8 178.24(3) . . ?
I8 Pb4 I8 89.49(4) 6 . ?
Pb1 I1 Pb2 77.14(4) . . ?
Pb1 I2 Pb2 77.78(3) . . ?
Pb1 I2 K2 87.78(5) . 3_546 ?
Pb2 I2 K2 83.23(5) . 3_546 ?
Pb2 I3 Pb3 93.18(3) . . ?
Pb2 I3 Pb3 93.18(3) . 6 ?
Pb3 I3 Pb3 101.44(4) . 6 ?
Pb2 I3 K2 86.46(7) . 3_546 ?
Pb3 I3 K2 129.263(18) . 3_546 ?
Pb3 I3 K2 129.261(18) 6 3_546 ?
Pb2 I3 K3 150.18(11) . . ?
Pb3 I3 K3 105.39(7) . . ?
Pb3 I3 K3 105.39(7) 6 . ?
K2 I3 K3 63.72(13) 3_546 . ?
Pb2 I4 Pb3 92.97(3) . . ?
Pb2 I4 K1 90.08(5) . . ?
Pb3 I4 K1 107.39(9) . . ?
Pb3 I5 Pb3 98.26(4) . 6 ?
Pb3 I8 Pb4 92.41(3) . . ?
Pb4 I10 Pb4 86.99(4) . 5 ?
C3 N1 C7 120.1(10) . . ?
C3 N1 C2 119.8(10) . . ?
C7 N1 C2 119.3(10) . . ?
C10 N2 C11 120.2(10) . . ?
C10 N2 C13 121.3(10) . . ?
C11 N2 C13 117.9(10) . . ?
O2 C1 O1 127.3(10) . . ?
O2 C1 C2 117.3(10) . . ?
O1 C1 C2 115.4(10) . . ?
N1 C2 C1 110.6(9) . . ?
N1 C3 C4 120.3(12) . . ?
C5 C4 C3 121.0(11) . . ?
C4 C5 C6 117.6(11) . . ?
C4 C5 C8 121.9(11) . . ?
C6 C5 C8 120.5(10) . . ?
C7 C6 C5 119.6(11) . . ?
C6 C7 N1 121.4(11) . . ?
C9 C8 C12 116.8(11) . . ?
C9 C8 C5 122.4(11) . . ?
C12 C8 C5 120.7(10) . . ?
C10 C9 C8 120.6(12) . . ?
C9 C10 N2 121.9(11) . . ?
C12 C11 N2 120.1(11) . . ?
C11 C12 C8 120.4(11) . . ?
N2 C13 C14 110.2(9) . . ?
O3 C14 O4 128.2(10) . . ?
O3 C14 C13 119.2(10) . . ?
O4 C14 C13 112.6(10) . . ?
C1 O1 Ni1 123.4(7) . . ?
C1 O1 K1 140.8(7) . . ?
Ni1 O1 K1 91.1(3) . . ?
C14 O4 Ni1 124.5(7) . 3_455 ?
C14 O4 K2 138.0(6) . . ?
Ni1 O4 K2 92.3(3) 3_455 . ?
K2 O5 K3 89.9(3) . 3_454 ?
Ni1 O6 K1 90.8(4) . . ?
Ni1 O7 K2 87.8(3) . 3_545 ?
O1 K1 O1 60.9(3) . 6 ?
O1 K1 O6 63.1(2) . . ?
O1 K1 O6 63.1(2) 6 . ?
O1 K1 O9 125.1(4) . . ?
O1 K1 O9 125.1(4) 6 . ?
O6 K1 O9 73.5(5) . . ?
O1 K1 O11 65.9(4) . 8 ?
O1 K1 O11 118.0(4) 6 8 ?
O6 K1 O11 66.0(4) . 8 ?
O9 K1 O11 66.7(4) . 8 ?
O1 K1 O11 118.0(4) . 3_545 ?
O1 K1 O11 65.9(4) 6 3_545 ?
O6 K1 O11 66.0(4) . 3_545 ?
O9 K1 O11 66.7(4) . 3_545 ?
O11 K1 O11 119.9(9) 8 3_545 ?
O1 K1 Ni1 36.72(16) . . ?
O1 K1 Ni1 36.73(16) 6 . ?
O6 K1 Ni1 36.7(2) . . ?
O9 K1 Ni1 110.2(5) . . ?
O11 K1 Ni1 81.3(3) 8 . ?
O11 K1 Ni1 81.3(3) 3_545 . ?
O1 K1 I4 154.5(2) . 6 ?
O1 K1 I4 103.39(16) 6 6 ?
O6 K1 I4 130.55(14) . 6 ?
O9 K1 I4 80.1(4) . 6 ?
O11 K1 I4 136.8(3) 8 6 ?
O11 K1 I4 65.3(4) 3_545 6 ?
Ni1 K1 I4 138.04(5) . 6 ?
O1 K1 I4 103.39(16) . . ?
O1 K1 I4 154.5(2) 6 . ?
O6 K1 I4 130.55(14) . . ?
O9 K1 I4 80.1(4) . . ?
O11 K1 I4 65.3(4) 8 . ?
O11 K1 I4 136.8(3) 3_545 . ?
Ni1 K1 I4 138.04(5) . . ?
I4 K1 I4 82.97(9) 6 . ?
O4 K2 O4 64.6(3) . 6_565 ?
O4 K2 O5 135.1(3) . . ?
O4 K2 O5 87.0(2) 6_565 . ?
O4 K2 O5 87.0(2) . 6_565 ?
O4 K2 O5 135.1(3) 6_565 6_565 ?
O5 K2 O5 90.7(4) . 6_565 ?
O4 K2 O7 60.4(2) . 3_455 ?
O4 K2 O7 60.4(2) 6_565 3_455 ?
O5 K2 O7 75.6(2) . 3_455 ?
O5 K2 O7 75.6(2) 6_565 3_455 ?
O4 K2 Ni1 36.15(15) . 3_455 ?
O4 K2 Ni1 36.15(15) 6_565 3_455 ?
O5 K2 Ni1 101.4(2) . 3_455 ?
O5 K2 Ni1 101.4(2) 6_565 3_455 ?
O7 K2 Ni1 37.10(19) 3_455 3_455 ?
O4 K2 I3 147.46(16) . 3_454 ?
O4 K2 I3 147.46(16) 6_565 3_454 ?
O5 K2 I3 64.49(19) . 3_454 ?
O5 K2 I3 64.50(19) 6_565 3_454 ?
O7 K2 I3 121.5(2) 3_455 3_454 ?
Ni1 K2 I3 158.61(12) 3_455 3_454 ?
O4 K2 I2 126.71(19) . 3_454 ?
O4 K2 I2 89.17(16) 6_565 3_454 ?
O5 K2 I2 83.9(2) . 3_454 ?
O5 K2 I2 135.1(2) 6_565 3_454 ?
O7 K2 I2 143.62(6) 3_455 3_454 ?
Ni1 K2 I2 123.33(8) 3_455 3_454 ?
I3 K2 I2 73.16(6) 3_454 3_454 ?
O4 K2 I2 89.17(16) . 8_454 ?
O4 K2 I2 126.71(19) 6_565 8_454 ?
O5 K2 I2 135.1(2) . 8_454 ?
O5 K2 I2 83.9(2) 6_565 8_454 ?
O7 K2 I2 143.62(6) 3_455 8_454 ?
Ni1 K2 I2 123.33(8) 3_455 8_454 ?
I3 K2 I2 73.16(6) 3_454 8_454 ?
I2 K2 I2 69.91(7) 3_454 8_454 ?
O4 K2 K3 111.3(2) . 3_454 ?
O4 K2 K3 111.3(2) 6_565 3_454 ?
O5 K2 K3 45.9(2) . 3_454 ?
O5 K2 K3 45.9(2) 6_565 3_454 ?
O7 K2 K3 61.1(2) 3_455 3_454 ?
Ni1 K2 K3 98.24(14) 3_455 3_454 ?
I3 K2 K3 60.37(12) 3_454 3_454 ?
I2 K2 K3 121.55(11) 3_454 3_454 ?
I2 K2 K3 121.55(11) 8_454 3_454 ?
O8 K3 O5 133.6(2) . 3_546 ?
O8 K3 O5 133.6(2) . 8_556 ?
O5 K3 O5 87.3(4) 3_546 8_556 ?
O8 K3 O10 77.9(6) . 6 ?
O5 K3 O10 137.3(5) 3_546 6 ?
O5 K3 O10 83.5(6) 8_556 6 ?
O8 K3 O10 77.9(6) . . ?
O5 K3 O10 83.5(6) 3_546 . ?
O5 K3 O10 137.3(5) 8_556 . ?
O10 K3 O10 75.9(8) 6 . ?
O8 K3 I3 114.1(4) . . ?
O5 K3 I3 61.2(2) 3_546 . ?
O5 K3 I3 61.2(2) 8_556 . ?
O10 K3 I3 141.2(5) 6 . ?
O10 K3 I3 141.2(5) . . ?
O8 K3 K2 170.0(4) . 3_546 ?
O5 K3 K2 44.2(2) 3_546 3_546 ?
O5 K3 K2 44.2(2) 8_556 3_546 ?
O10 K3 K2 109.7(6) 6 3_546 ?
O10 K3 K2 109.7(6) . 3_546 ?
I3 K3 K2 55.91(10) . 3_546 ?

_refine_diff_density_max         1.369
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.250


