Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Chaudhuri, N. R.'
'Maji, Tapas Kumar'
'Mostafa, G.'
'Mukherjee, Partha Sarathi'
'Zangrando, Ennio'

_publ_contact_author_name     	'Dr N R Chaudhuri'  
_publ_contact_author_address 
;
Dr N R Chaudhuri
Department of Inorganic Chemistry
Indian Association for the Cultivation of Science
Calcutta
700 032
INDIA
;

_publ_contact_author_email       'icnrc@mahendra.iacs.res.in'


data_1
_database_code_CSD                  154468

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
catena-bis(3-aminopropyl)methylamine-copper(II)
-tetra-cyanonickel(II) diperchlorate solvated
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
'[(C7 H19 N3 Cu)2 Ni(CN)4 2+] 2(Cl O4 1-) 2.5(H2 O)'  
_chemical_formula_sum     
'C18 H43 Cl2 Cu2 N10 Ni O10.50'
_chemical_formula_weight          824.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0181   0.0091
'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'
'Cl'  'Cl'   0.3639   0.7018
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu'  'Cu'  -1.9646   0.5888
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N'  'N'   0.0311   0.0180
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ni'  'Ni'  -3.0029   0.5091
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0492   0.0322
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            'monoclinic'
_symmetry_space_group_name_H-M    'P21/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                    7.806(2)
_cell_length_b                    14.619(7)
_cell_length_c                    15.069(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  97.41(2)
_cell_angle_gamma                 90.00
_cell_volume                      1705.3(11)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       10
_cell_measurement_theta_max       30

_exptl_crystal_description        'parallelopiped'  
_exptl_crystal_colour             'deep blue'   
_exptl_crystal_size_max           0.42   
_exptl_crystal_size_mid           0.25   
_exptl_crystal_size_min           0.11   
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.605
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              850
_exptl_absorpt_coefficient_mu     4.075
_exptl_absorpt_correction_type    'psi-scan'
_exptl_absorpt_correction_T_min   0.6767   
_exptl_absorpt_correction_T_max   0.9979   
_exptl_absorpt_process_details    'psi scan method'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(2)   
_diffrn_radiation_wavelength      1.54180   
_diffrn_radiation_type            CuK\a   
_diffrn_radiation_source          'fine-focus sealed tube'  
_diffrn_radiation_monochromator   graphite   
_diffrn_measurement_device        'Enraf-Nonius CAD4 diffractometer'   
_diffrn_measurement_method        \w-2\q   
_diffrn_standards_number          3   
_diffrn_standards_interval_count  100   
_diffrn_standards_interval_time   ?   
_diffrn_standards_decay_%         1.9   
_diffrn_reflns_number             3402
_diffrn_reflns_av_R_equivalents   0.0165
_diffrn_reflns_av_sigmaI/netI     0.0142
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          75.03
_reflns_number_total              3247
_reflns_number_gt                 2960
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        ?   
_computing_cell_refinement        ?   
_computing_data_reduction         ?   
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'   
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'   
_computing_molecular_graphics     'ORTEX (P.McArdle, 1995)'   
_computing_publication_material   'SHELXL-97/2 (Sheldrick,1997)'   
_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1063P)^2^+1.9708P] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      Patterson
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0028(4)
_refine_ls_extinction_expression
'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3247
_refine_ls_number_parameters      247
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0597
_refine_ls_R_factor_gt            0.0559
_refine_ls_wR_factor_ref          0.1712
_refine_ls_wR_factor_gt           0.1672
_refine_ls_goodness_of_fit_ref    1.088
_refine_ls_restrained_S_all       1.088
_refine_ls_shift/su_max           0.004
_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
Ni Ni 0.55443(10) 0.2500 -0.03714(5) 0.0336(3) Uani 1 2 d S . .
Cu Cu 0.76437(6) 0.01604(4) 0.19407(3) 0.0385(2) Uani 1 1 d . . .
N1 N 0.6158(4) 0.0854(3) 0.2693(2) 0.0550(9) Uani 1 1 d . . .
H1A H 0.6769 0.1339 0.2926 0.066 Uiso 1 1 calc R . .
H1B H 0.5249 0.1075 0.2328 0.066 Uiso 1 1 calc R . .
N2 N 0.9100(4) -0.0399(3) 0.3056(2) 0.0467(8) Uani 1 1 d . . .
N3 N 0.9283(5) -0.0239(3) 0.1084(3) 0.0659(11) Uani 1 1 d . . .
H3A H 0.8672 -0.0253 0.0536 0.079 Uiso 1 1 calc R . .
H3B H 1.0072 0.0209 0.1076 0.079 Uiso 1 1 calc R . .
N4 N 0.6815(5) 0.1062(3) 0.0963(2) 0.0549(9) Uani 1 1 d . . .
N5 N 0.4090(5) 0.0995(3) -0.1592(2) 0.0532(9) Uani 1 1 d . . .
C1 C 0.5489(6) 0.0379(4) 0.3425(3) 0.0662(13) Uani 1 1 d . . .
H1C H 0.4782 -0.0133 0.3189 0.079 Uiso 1 1 calc R . .
H1D H 0.4766 0.0793 0.3717 0.079 Uiso 1 1 calc R . .
C2 C 0.6946(7) 0.0035(4) 0.4102(3) 0.0689(14) Uani 1 1 d . . .
H2A H 0.7682 0.0547 0.4307 0.083 Uiso 1 1 calc R . .
H2B H 0.6461 -0.0206 0.4614 0.083 Uiso 1 1 calc R . .
C3 C 0.8028(7) -0.0688(4) 0.3753(3) 0.0633(12) Uani 1 1 d . . .
H3C H 0.8790 -0.0939 0.4253 0.076 Uiso 1 1 calc R . .
H3D H 0.7272 -0.1178 0.3509 0.076 Uiso 1 1 calc R . .
C4 C 1.0033(8) -0.1249(4) 0.2839(4) 0.0732(15) Uani 1 1 d . . .
H4A H 0.9179 -0.1717 0.2657 0.088 Uiso 1 1 calc R . .
H4B H 1.0720 -0.1460 0.3382 0.088 Uiso 1 1 calc R . .
C5 C 1.1200(8) -0.1166(5) 0.2121(4) 0.0829(18) Uani 1 1 d . . .
H5A H 1.1922 -0.0628 0.2238 0.099 Uiso 1 1 calc R . .
H5B H 1.1953 -0.1696 0.2148 0.099 Uiso 1 1 calc R . .
C6 C 1.0231(8) -0.1095(5) 0.1196(4) 0.0832(18) Uani 1 1 d . . .
H6A H 1.1038 -0.1131 0.0759 0.100 Uiso 1 1 calc R . .
H6B H 0.9432 -0.1603 0.1093 0.100 Uiso 1 1 calc R . .
C7 C 1.0378(6) 0.0291(4) 0.3419(4) 0.0726(15) Uani 1 1 d . . .
H7A H 1.1046 0.0479 0.2958 0.109 Uiso 1 1 calc R . .
H7B H 1.1131 0.0032 0.3909 0.109 Uiso 1 1 calc R . .
H7C H 0.9791 0.0811 0.3625 0.109 Uiso 1 1 calc R . .
C8 C 0.6373(5) 0.1606(3) 0.0452(2) 0.0434(8) Uani 1 1 d . . .
C9 C 0.4668(4) 0.1586(3) -0.1154(2) 0.0413(8) Uani 1 1 d . . .
O1W O 0.2652(10) 0.0456(7) 0.0773(6) 0.077(2) Uani 0.50 1 d P . .
O3WB O 0.8203(18) 0.2500 0.3686(7) 0.068(3) Uani 0.50 2 d SP . .
O3W O 0.832(2) 0.2500 0.303(2) 0.151(9) Uani 0.50 2 d SP . .
O2W O 0.1755(14) 0.2500 0.3821(9) 0.095(4) Uani 0.50 2 d SP . .
Cl1A Cl 0.5788(3) 0.2500 0.55646(18) 0.0928(7) Uani 1 2 d S . .
O11A O 0.567(2) 0.2500 0.6485(8) 0.271(10) Uani 1 2 d S . .
O12A O 0.735(2) 0.2500 0.5318(9) 0.257(9) Uani 1 2 d S . .
O13A O 0.607(2) 0.1601(9) 0.5625(10) 0.138(5) Uani 0.50 1 d P . .
O14A O 0.441(3) 0.2846(11) 0.5051(15) 0.253(12) Uani 0.50 1 d P . .
Cl1B Cl 0.2053(3) 0.2120(2) 0.1364(2) 0.0906(10) Uani 0.50 1 d P . .
O11B O 0.3328(12) 0.2500 0.2021(7) 0.153(4) Uani 1 2 d S . .
O12B O 0.2190(14) 0.2500 0.0557(6) 0.138(3) Uani 1 2 d S . .
O13B O 0.0457(12) 0.2142(9) 0.1596(10) 0.142(6) Uani 0.50 1 d P . .
O14B O 0.2415(19) 0.1154(10) 0.1214(17) 0.214(11) Uani 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0378(4) 0.0354(5) 0.0250(4) 0.000 -0.0057(3) 0.000
Cu 0.0403(3) 0.0432(4) 0.0294(3) 0.00401(19) -0.0056(2) 0.0008(2)
N1 0.0543(18) 0.063(3) 0.0440(17) -0.0035(16) -0.0074(13) 0.0125(17)
N2 0.0480(16) 0.052(2) 0.0367(15) 0.0068(14) -0.0077(12) 0.0047(15)
N3 0.062(2) 0.094(3) 0.0434(18) 0.010(2) 0.0120(15) 0.014(2)
N4 0.067(2) 0.053(2) 0.0416(17) 0.0104(16) -0.0060(15) 0.0029(17)
N5 0.063(2) 0.051(2) 0.0433(17) -0.0092(15) -0.0024(14) -0.0139(16)
C1 0.056(2) 0.093(4) 0.050(2) -0.010(2) 0.0103(18) 0.007(2)
C2 0.083(3) 0.089(4) 0.036(2) 0.000(2) 0.010(2) 0.005(3)
C3 0.081(3) 0.069(3) 0.039(2) 0.016(2) 0.0023(19) 0.007(2)
C4 0.084(3) 0.066(4) 0.067(3) 0.015(3) -0.002(2) 0.030(3)
C5 0.075(3) 0.089(4) 0.085(4) 0.009(3) 0.012(3) 0.042(3)
C6 0.079(3) 0.102(5) 0.071(3) -0.005(3) 0.018(3) 0.033(3)
C7 0.058(3) 0.085(4) 0.067(3) 0.000(3) -0.024(2) -0.008(2)
C8 0.0465(18) 0.046(2) 0.0352(17) -0.0004(16) -0.0060(13) -0.0001(16)
C9 0.0427(17) 0.048(2) 0.0313(15) 0.0022(15) -0.0036(12) -0.0026(15)
O1W 0.071(4) 0.065(5) 0.094(6) 0.007(4) 0.006(4) -0.009(4)
O3WB 0.089(7) 0.054(7) 0.061(6) 0.000 0.006(6) 0.000
O3W 0.105(12) 0.055(9) 0.27(3) 0.000 -0.041(17) 0.000
O2W 0.055(6) 0.119(11) 0.101(9) 0.000 -0.021(5) 0.000
Cl1A 0.0933(15) 0.0862(18) 0.0901(15) 0.000 -0.0213(12) 0.000
O11A 0.247(16) 0.46(3) 0.091(7) 0.000 -0.014(8) 0.000
O12A 0.204(14) 0.43(3) 0.136(10) 0.000 0.034(9) 0.000
O13A 0.177(12) 0.083(9) 0.155(12) 0.006(8) 0.021(9) 0.026(8)
O14A 0.27(2) 0.14(2) 0.30(2) -0.010(14) -0.154(18) 0.064(14)
Cl1B 0.0586(13) 0.106(3) 0.102(2) 0.0347(17) -0.0073(12) -0.0134(12)
O11B 0.108(6) 0.207(11) 0.130(7) 0.000 -0.037(5) 0.000
O12B 0.171(8) 0.137(8) 0.096(6) 0.000 -0.016(5) 0.000
O13B 0.076(5) 0.158(17) 0.198(12) 0.001(9) 0.034(6) -0.004(6)
O14B 0.130(10) 0.085(10) 0.41(3) 0.100(15) -0.014(14) -0.031(8)

_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
Ni C9 1.854(4) . ?
Ni C9 1.854(4) 4_565 ?
Ni C8 1.860(4) 4_565 ?
Ni C8 1.860(4) . ?
Cu N1 2.000(4) . ?
Cu N3 2.018(4) . ?
Cu N4 2.020(4) . ?
Cu N2 2.072(3) . ?
Cu N5 2.186(4) 3_655 ?
N1 C1 1.456(6) . ?
N2 C7 1.473(6) . ?
N2 C3 1.486(6) . ?
N2 C4 1.497(6) . ?
N3 C6 1.452(7) . ?
N4 C8 1.130(5) . ?
N5 C9 1.143(5) . ?
N5 Cu 2.186(4) 3_655 ?
C1 C2 1.512(7) . ?
C2 C3 1.490(7) . ?
C4 C5 1.507(8) . ?
C5 C6 1.500(8) . ?
O1W O14B 1.24(2) . ?
O3WB O3W 1.01(3) . ?
Cl1A O12A 1.320(16) . ?
Cl1A O13A 1.333(13) 4_565 ?
Cl1A O13A 1.333(13) . ?
Cl1A O14A 1.339(14) 4_565 ?
Cl1A O14A 1.339(14) . ?
Cl1A O11A 1.402(12) . ?
O12A O13A 1.751(16) . ?
O12A O13A 1.751(16) 4_565 ?
O13A O14A 1.67(2) 4_565 ?
O14A O14A 1.01(3) 4_565 ?
O14A O13A 1.67(2) 4_565 ?
Cl1B Cl1B 1.110(7) 4_565 ?
Cl1B O13B 1.337(10) . ?
Cl1B O12B 1.354(9) . ?
Cl1B O11B 1.422(8) . ?
Cl1B O14B 1.463(18) . ?
Cl1B O13B 1.717(11) 4_565 ?
O11B Cl1B 1.422(8) 4_565 ?
O12B Cl1B 1.354(9) 4_565 ?
O13B O13B 1.05(3) 4_565 ?
O13B Cl1B 1.717(11) 4_565 ?

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
C9 Ni C9 92.3(2) . 4_565 ?
C9 Ni C8 177.48(17) . 4_565 ?
C9 Ni C8 89.20(17) 4_565 4_565 ?
C9 Ni C8 89.20(17) . . ?
C9 Ni C8 177.48(17) 4_565 . ?
C8 Ni C8 89.3(2) 4_565 . ?
N1 Cu N3 166.32(19) . . ?
N1 Cu N4 85.85(16) . . ?
N3 Cu N4 83.83(17) . . ?
N1 Cu N2 92.18(14) . . ?
N3 Cu N2 94.45(15) . . ?
N4 Cu N2 160.01(15) . . ?
N1 Cu N5 98.16(16) . 3_655 ?
N3 Cu N5 92.68(18) . 3_655 ?
N4 Cu N5 101.46(15) . 3_655 ?
N2 Cu N5 98.51(14) . 3_655 ?
C1 N1 Cu 118.6(3) . . ?
C7 N2 C3 110.4(4) . . ?
C7 N2 C4 108.9(4) . . ?
C3 N2 C4 104.7(4) . . ?
C7 N2 Cu 107.8(3) . . ?
C3 N2 Cu 112.7(2) . . ?
C4 N2 Cu 112.4(3) . . ?
C6 N3 Cu 122.1(3) . . ?
C8 N4 Cu 176.0(4) . . ?
C9 N5 Cu 155.3(3) . 3_655 ?
N1 C1 C2 110.9(4) . . ?
C3 C2 C1 114.2(4) . . ?
N2 C3 C2 116.4(4) . . ?
N2 C4 C5 116.6(5) . . ?
C6 C5 C4 113.1(5) . . ?
N3 C6 C5 110.9(5) . . ?
N4 C8 Ni 177.3(4) . . ?
N5 C9 Ni 175.7(3) . . ?
O12A Cl1A O13A 82.6(7) . 4_565 ?
O12A Cl1A O13A 82.6(7) . . ?
O13A Cl1A O13A 160.6(14) 4_565 . ?
O12A Cl1A O14A 122.6(14) . 4_565 ?
O13A Cl1A O14A 121.5(10) 4_565 4_565 ?
O13A Cl1A O14A 77.3(9) . 4_565 ?
O12A Cl1A O14A 122.6(14) . . ?
O13A Cl1A O14A 77.3(9) 4_565 . ?
O13A Cl1A O14A 121.5(11) . . ?
O14A Cl1A O14A 44.3(14) 4_565 . ?
O12A Cl1A O11A 117.2(9) . . ?
O13A Cl1A O11A 87.9(7) 4_565 . ?
O13A Cl1A O11A 87.9(7) . . ?
O14A Cl1A O11A 115.1(14) 4_565 . ?
O14A Cl1A O11A 115.1(14) . . ?
O13B Cl1B O12B 114.1(8) . . ?
O13B Cl1B O11B 113.7(8) . . ?
O12B Cl1B O11B 109.6(6) . . ?
O13B Cl1B O14B 105.5(9) . . ?
O12B Cl1B O14B 102.6(10) . . ?
O11B Cl1B O14B 110.6(7) . . ?
O13B Cl1B O13B 37.6(9) . 4_565 ?
O12B Cl1B O13B 93.9(6) . 4_565 ?
O11B Cl1B O13B 94.3(6) . 4_565 ?
O14B Cl1B O13B 142.8(7) . 4_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Cu N1 C1 -165.1(6) . . . . ?
N4 Cu N1 C1 153.8(3) . . . . ?
N2 Cu N1 C1 -46.1(3) . . . . ?
N5 Cu N1 C1 52.8(3) 3_655 . . . ?
N1 Cu N2 C7 -80.6(3) . . . . ?
N3 Cu N2 C7 87.4(4) . . . . ?
N4 Cu N2 C7 3.2(6) . . . . ?
N5 Cu N2 C7 -179.2(3) 3_655 . . . ?
N1 Cu N2 C3 41.4(3) . . . . ?
N3 Cu N2 C3 -150.6(3) . . . . ?
N4 Cu N2 C3 125.2(5) . . . . ?
N5 Cu N2 C3 -57.2(3) 3_655 . . . ?
N1 Cu N2 C4 159.3(3) . . . . ?
N3 Cu N2 C4 -32.6(4) . . . . ?
N4 Cu N2 C4 -116.8(5) . . . . ?
N5 Cu N2 C4 60.8(3) 3_655 . . . ?
N1 Cu N3 C6 153.6(6) . . . . ?
N4 Cu N3 C6 -165.2(5) . . . . ?
N2 Cu N3 C6 34.8(5) . . . . ?
N5 Cu N3 C6 -63.9(5) 3_655 . . . ?
N1 Cu N4 C8 48(5) . . . . ?
N3 Cu N4 C8 -123(5) . . . . ?
N2 Cu N4 C8 -37(6) . . . . ?
N5 Cu N4 C8 146(5) 3_655 . . . ?
Cu N1 C1 C2 60.9(5) . . . . ?
N1 C1 C2 C3 -65.7(6) . . . . ?
C7 N2 C3 C2 62.8(5) . . . . ?
C4 N2 C3 C2 179.9(4) . . . . ?
Cu N2 C3 C2 -57.7(5) . . . . ?
C1 C2 C3 N2 67.7(6) . . . . ?
C7 N2 C4 C5 -63.5(6) . . . . ?
C3 N2 C4 C5 178.4(5) . . . . ?
Cu N2 C4 C5 55.8(6) . . . . ?
N2 C4 C5 C6 -73.7(8) . . . . ?
Cu N3 C6 C5 -53.0(7) . . . . ?
C4 C5 C6 N3 67.2(8) . . . . ?
Cu N4 C8 Ni -87(10) . . . . ?
C9 Ni C8 N4 -84(8) . . . . ?
C9 Ni C8 N4 42(10) 4_565 . . . ?
C8 Ni C8 N4 94(8) 4_565 . . . ?
Cu N5 C9 Ni 22(5) 3_655 . . . ?
C9 Ni C9 N5 -134(5) 4_565 . . . ?
C8 Ni C9 N5 -8(7) 4_565 . . . ?
C8 Ni C9 N5 44(5) . . . . ?


_diffrn_measured_fraction_theta_max    0.889
_diffrn_reflns_theta_full              75.03
_diffrn_measured_fraction_theta_full   0.889
_refine_diff_density_max    1.086
_refine_diff_density_min   -0.700
_refine_diff_density_rms    0.105

#======END
data_2
_database_code_CSD                  163231

_audit_creation_method            SHELXL-97

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
catena-bis(3-aminopropyl)methylamine-copper(II)
-tetra-cyanonickel(II) diperchlorate 
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
'[(C7 H19 N3 Cu)2 Ni(CN)4 2+] 2(Cl O4 1-)'  

_chemical_formula_sum
'C18 H38 Cl2 Cu2 N10 Ni O8'
_chemical_formula_weight          779.27

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'
'Cl'  'Cl'   0.1484   0.1585
'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'
'Cu'  'Cu'   0.3201   1.2651
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting   'monoclinic '
_symmetry_space_group_name_H-M   'P21/c'  

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

_cell_length_a                    14.410(6)
_cell_length_b                    14.154(4)
_cell_length_c                    16.014(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.86(2)
_cell_angle_gamma                 90.00
_cell_volume                      3264.5(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        'parallelopiped'  
_exptl_crystal_colour             'deep blue'   
_exptl_crystal_size_max           0.40   
_exptl_crystal_size_mid           0.20   
_exptl_crystal_size_min           0.15  
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.586
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1600
_exptl_absorpt_coefficient_mu     2.080
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min      0.7770
_exptl_absorpt_correction_T_max      1.1094
_exptl_absorpt_process_details    ?
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(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   'image plate dip1030'
_diffrn_measurement_method        'laser scanner'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9590
_diffrn_reflns_av_R_equivalents   0.0650
_diffrn_reflns_av_sigmaI/netI     0.0774
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.36
_diffrn_reflns_theta_max          23.96
_reflns_number_total              5016
_reflns_number_gt                 3108
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Nonius Xpress'
_computing_cell_refinement        'MOSFLM (J. Appl. Cryst., 1993, 21, 67)'
_computing_data_reduction         'MOSFLM (J. Appl. Cryst., 1993, 21, 67)'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep3/Windows (Farrugia,1997)'
_computing_publication_material   'WinGX 1.63 (Farrugia, 1999)' 

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

PERCHLORATE ANIONS disordered: at Cl1 (occupancies of 0.66 and 0.34); 
at Cl2 (occupancies 0.63, 0.37) over two positions for a 30=B0 rotation 
about the Cl2-O6 bond. Lower occupancies isotropically, higher
anisotropically refined with same thermal factors.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1315P)^2^] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5016
_refine_ls_number_parameters      366
_refine_ls_number_restraints      60
_refine_ls_R_factor_all           0.1075
_refine_ls_R_factor_gt            0.0690
_refine_ls_wR_factor_ref          0.2263
_refine_ls_wR_factor_gt           0.1983
_refine_ls_goodness_of_fit_ref    1.053
_refine_ls_restrained_S_all       1.070
_refine_ls_shift/su_max           0.021
_refine_ls_shift/su_mean          0.002

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
Ni Ni 0.52270(7) 0.29172(7) 0.74551(6) 0.0690(4) Uani 1 1 d . . .
Cu1 Cu 0.70540(7) 0.02577(7) 0.87787(6) 0.0729(4) Uani 1 1 d . . .
Cu2 Cu 0.31274(7) 0.06128(7) 0.59451(6) 0.0754(4) Uani 1 1 d . . .
N1 N 0.8037(5) -0.0389(5) 0.8123(5) 0.095(2) Uani 1 1 d . . .
H1A H 0.8308 -0.0830 0.8454 0.114 Uiso 1 1 calc R . .
H1B H 0.7753 -0.0694 0.7693 0.114 Uiso 1 1 calc R . .
N2 N 0.8050(5) 0.0918(5) 0.9519(4) 0.083(2) Uani 1 1 d . . .
N3 N 0.6021(6) 0.0496(6) 0.9575(5) 0.106(3) Uani 1 1 d . . .
H3A H 0.5484 0.0466 0.9273 0.127 Uiso 1 1 calc R . .
H3B H 0.6020 0.0006 0.9934 0.127 Uiso 1 1 calc R . .
N4 N 0.4089(6) 0.1508(6) 0.6471(5) 0.093(2) Uani 1 1 d . . .
N5 N 0.6199(5) 0.4336(5) 0.8607(5) 0.086(2) Uani 1 1 d . . .
N1A N 0.2374(6) 0.0843(7) 0.6943(5) 0.107(3) Uani 1 1 d . . .
H1A1 H 0.2766 0.1029 0.7361 0.128 Uiso 1 1 calc R . .
H1A2 H 0.1996 0.1335 0.6825 0.128 Uiso 1 1 calc R . .
N2A N 0.2031(5) -0.0041(6) 0.5305(4) 0.087(2) Uani 1 1 d . . .
N3A N 0.3829(6) 0.0792(6) 0.4883(5) 0.108(3) Uani 1 1 d . . .
H3A1 H 0.3583 0.1302 0.4623 0.129 Uiso 1 1 calc R . .
H3A2 H 0.4416 0.0944 0.5037 0.129 Uiso 1 1 calc R . .
N4A N 0.3868(5) 0.4372(5) 0.6815(4) 0.086(2) Uani 1 1 d . . .
N5A N 0.6672(5) 0.1479(5) 0.7986(4) 0.0801(19) Uani 1 1 d . . .
C1 C 0.8773(7) 0.0202(9) 0.7786(7) 0.113(3) Uani 1 1 d . . .
H1C H 0.8495 0.0673 0.7415 0.135 Uiso 1 1 calc R . .
H1D H 0.9179 -0.0189 0.7461 0.135 Uiso 1 1 calc R . .
C2 C 0.9344(7) 0.0697(9) 0.8474(7) 0.116(4) Uani 1 1 d . . .
H2A H 0.9634 0.0219 0.8830 0.139 Uiso 1 1 calc R . .
H2B H 0.9836 0.1051 0.8219 0.139 Uiso 1 1 calc R . .
C3 C 0.8817(7) 0.1348(8) 0.9006(7) 0.102(3) Uani 1 1 d . . .
H3C H 0.8541 0.1833 0.8649 0.123 Uiso 1 1 calc R . .
H3D H 0.9255 0.1659 0.9388 0.123 Uiso 1 1 calc R . .
C4 C 0.7685(8) 0.1741(8) 1.0004(7) 0.107(3) Uani 1 1 d . . .
H4A H 0.7468 0.2222 0.9612 0.128 Uiso 1 1 calc R . .
H4B H 0.8193 0.2011 1.0338 0.128 Uiso 1 1 calc R . .
C5 C 0.6897(10) 0.1493(10) 1.0578(7) 0.130(4) Uani 1 1 d . . .
H5A H 0.6820 0.1998 1.0979 0.156 Uiso 1 1 calc R . .
H5B H 0.7051 0.0920 1.0884 0.156 Uiso 1 1 calc R . .
C6 C 0.5988(8) 0.1349(8) 1.0072(7) 0.114(3) Uani 1 1 d . . .
H6A H 0.5477 0.1309 1.0450 0.136 Uiso 1 1 calc R . .
H6B H 0.5879 0.1888 0.9708 0.136 Uiso 1 1 calc R . .
C7 C 0.8452(8) 0.0164(8) 1.0111(7) 0.119(4) Uani 1 1 d . . .
H7A H 0.8900 0.0448 1.0491 0.178 Uiso 1 1 calc R . .
H7B H 0.8748 -0.0318 0.9793 0.178 Uiso 1 1 calc R . .
H7C H 0.7962 -0.0111 1.0422 0.178 Uiso 1 1 calc R . .
C8 C 0.4371(6) 0.3834(6) 0.7080(5) 0.075(2) Uani 1 1 d . . .
C9 C 0.5845(6) 0.3801(6) 0.8151(5) 0.075(2) Uani 1 1 d . . .
C1A C 0.1801(9) 0.0081(10) 0.7266(7) 0.124(4) Uani 1 1 d . . .
H1A3 H 0.1482 0.0303 0.7753 0.149 Uiso 1 1 calc R . .
H1A4 H 0.2195 -0.0445 0.7438 0.149 Uiso 1 1 calc R . .
C2A C 0.1087(8) -0.0255(10) 0.6604(8) 0.128(4) Uani 1 1 d . . .
H2A1 H 0.0668 -0.0701 0.6856 0.153 Uiso 1 1 calc R . .
H2A2 H 0.0723 0.0281 0.6407 0.153 Uiso 1 1 calc R . .
C3A C 0.1525(7) -0.0714(8) 0.5879(7) 0.111(3) Uani 1 1 d . . .
H3A3 H 0.1046 -0.1041 0.5551 0.133 Uiso 1 1 calc R . .
H3A4 H 0.1963 -0.1185 0.6087 0.133 Uiso 1 1 calc R . .
C4A C 0.2363(7) -0.0688(8) 0.4647(7) 0.110(3) Uani 1 1 d . . .
H4A1 H 0.1829 -0.0997 0.4385 0.132 Uiso 1 1 calc R . .
H4A2 H 0.2743 -0.1175 0.4914 0.132 Uiso 1 1 calc R . .
C5A C 0.2932(8) -0.0218(9) 0.3957(6) 0.114(4) Uani 1 1 d . . .
H5A1 H 0.2984 -0.0654 0.3493 0.137 Uiso 1 1 calc R . .
H5A2 H 0.2606 0.0340 0.3753 0.137 Uiso 1 1 calc R . .
C6A C 0.3881(7) 0.0057(8) 0.4268(6) 0.103(3) Uani 1 1 d . . .
H6A1 H 0.4193 -0.0489 0.4512 0.124 Uiso 1 1 calc R . .
H6A2 H 0.4241 0.0276 0.3804 0.124 Uiso 1 1 calc R . .
C7A C 0.1403(7) 0.0710(9) 0.4937(7) 0.122(4) Uani 1 1 d . . .
H7A1 H 0.0902 0.0418 0.4623 0.183 Uiso 1 1 calc R . .
H7A2 H 0.1749 0.1109 0.4576 0.183 Uiso 1 1 calc R . .
H7A3 H 0.1156 0.1083 0.5379 0.183 Uiso 1 1 calc R . .
C8A C 0.4553(6) 0.2032(6) 0.6826(5) 0.077(2) Uani 1 1 d . . .
C9A C 0.6122(6) 0.2026(5) 0.7771(5) 0.071(2) Uani 1 1 d . . .
Cl1 Cl 0.0040(2) 0.2611(2) 0.6565(2) 0.1192(10) Uani 1 1 d . . .
O1 O 0.0727(11) 0.2334(12) 0.7119(11) 0.198(6) Uani 0.658(19) 1 d PD . .
O2 O -0.0316(11) 0.1748(12) 0.6212(11) 0.198(6) Uani 0.658(19) 1 d PD . .
O3 O -0.0757(11) 0.2921(11) 0.6996(11) 0.198(6) Uani 0.658(19) 1 d PD . .
O4 O 0.0286(12) 0.3240(12) 0.6018(12) 0.198(6) Uani 0.658(19) 1 d PD . .
O1B O -0.0311(14) 0.3492(15) 0.6641(13) 0.103(8) Uiso 0.342(19) 1 d PD . .
O2B O -0.0392(18) 0.2069(16) 0.5886(16) 0.127(10) Uiso 0.342(19) 1 d PD . .=

O3B O 0.106(2) 0.274(2) 0.623(2) 0.201(17) Uiso 0.342(19) 1 d PD . .
O4B O 0.016(3) 0.207(2) 0.7276(19) 0.33(4) Uiso 0.342(19) 1 d PD . .
Cl2 Cl 0.3437(3) 0.1705(3) 0.9083(2) 0.1408(13) Uani 1 1 d . . .
O5 O 0.3310(8) 0.1653(8) 0.9918(5) 0.209(4) Uani 1 1 d D . .
O6 O 0.3923(16) 0.0832(14) 0.8862(11) 0.209(4) Uani 0.63(2) 1 d PD . .
O7 O 0.2525(13) 0.1482(17) 0.8726(9) 0.209(4) Uani 0.63(2) 1 d PD . .
O8 O 0.3774(19) 0.2406(14) 0.8766(10) 0.209(4) Uani 0.63(2) 1 d PD . .
O6B O 0.3632(17) 0.0894(16) 0.8675(15) 0.139(10) Uiso 0.37(2) 1 d PD . .
O7B O 0.2710(16) 0.222(2) 0.8650(15) 0.202(16) Uiso 0.37(2) 1 d PD . .
O8B O 0.4267(14) 0.2371(12) 0.9011(11) 0.096(7) Uiso 0.37(2) 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0717(7) 0.0678(7) 0.0668(6) -0.0025(4) -0.0104(5) 0.0011(5)
Cu1 0.0708(7) 0.0783(7) 0.0689(6) -0.0004(5) -0.0078(5) -0.0031(5)
Cu2 0.0811(7) 0.0751(7) 0.0689(6) -0.0009(5) -0.0138(5) -0.0032(5)
N1 0.084(5) 0.108(6) 0.092(5) -0.004(4) -0.014(4) 0.014(4)
N2 0.084(5) 0.082(5) 0.082(5) 0.000(4) -0.015(4) -0.008(4)
N3 0.099(6) 0.125(7) 0.095(6) -0.010(5) 0.019(5) -0.021(5)
N4 0.099(6) 0.087(5) 0.092(5) -0.005(4) -0.026(4) -0.004(4)
N5 0.096(5) 0.074(5) 0.087(5) -0.013(4) -0.023(4) -0.002(4)
N1A 0.108(6) 0.127(7) 0.084(5) -0.015(5) -0.005(5) -0.002(5)
N2A 0.066(5) 0.113(6) 0.081(5) -0.004(4) 0.003(4) -0.022(4)
N3A 0.130(7) 0.102(6) 0.090(5) 0.016(5) -0.011(5) -0.039(5)
N4A 0.085(5) 0.093(5) 0.080(5) 0.006(4) -0.008(4) 0.018(4)
N5A 0.079(5) 0.069(4) 0.091(5) 0.000(4) -0.012(4) 0.010(4)
C1 0.075(7) 0.154(10) 0.110(8) 0.001(7) 0.017(6) 0.007(7)
C2 0.074(7) 0.152(10) 0.121(9) 0.020(8) 0.002(6) 0.004(7)
C3 0.073(6) 0.126(9) 0.107(7) 0.021(6) -0.009(6) -0.020(6)
C4 0.117(9) 0.102(7) 0.100(7) -0.017(6) -0.014(6) -0.008(6)
C5 0.151(11) 0.147(11) 0.093(8) -0.036(7) 0.022(8) -0.011(9)
C6 0.114(9) 0.119(9) 0.109(8) -0.022(7) 0.037(7) -0.011(7)
C7 0.118(9) 0.135(9) 0.100(7) 0.023(6) -0.053(7) -0.013(7)
C8 0.079(6) 0.071(5) 0.074(5) 0.006(4) -0.007(4) 0.006(4)
C9 0.066(5) 0.082(6) 0.076(5) -0.002(4) -0.002(4) 0.003(4)
C1A 0.133(10) 0.161(11) 0.080(7) 0.005(7) 0.028(7) 0.041(9)
C2A 0.107(9) 0.165(12) 0.112(9) 0.015(8) 0.011(7) -0.010(8)
C3A 0.090(7) 0.134(9) 0.110(8) -0.017(7) 0.006(6) -0.021(6)
C4A 0.084(7) 0.137(9) 0.109(8) -0.051(7) 0.002(6) -0.021(6)
C5A 0.104(8) 0.163(10) 0.075(6) -0.030(6) 0.003(6) -0.012(7)
C6A 0.091(7) 0.137(9) 0.083(6) -0.003(6) 0.011(5) 0.004(6)
C7A 0.083(7) 0.181(11) 0.101(7) -0.005(7) -0.021(6) 0.039(7)
C8A 0.083(6) 0.070(5) 0.077(5) -0.004(4) -0.016(5) -0.005(4)
C9A 0.078(6) 0.068(5) 0.065(5) 0.000(4) -0.008(4) 0.006(4)
Cl1 0.117(2) 0.104(2) 0.135(2) 0.0107(18) -0.0178(19) 0.0049(17)
O1 0.162(9) 0.179(8) 0.249(12) 0.069(8) -0.056(8) -0.008(7)
O2 0.162(9) 0.179(8) 0.249(12) 0.069(8) -0.056(8) -0.008(7)
O3 0.162(9) 0.179(8) 0.249(12) 0.069(8) -0.056(8) -0.008(7)
O4 0.162(9) 0.179(8) 0.249(12) 0.069(8) -0.056(8) -0.008(7)
Cl2 0.186(4) 0.149(3) 0.0873(19) -0.0083(19) -0.005(2) -0.039(3)
O5 0.286(11) 0.218(8) 0.121(5) -0.013(5) -0.011(6) -0.071(8)
O6 0.286(11) 0.218(8) 0.121(5) -0.013(5) -0.011(6) -0.071(8)
O7 0.286(11) 0.218(8) 0.121(5) -0.013(5) -0.011(6) -0.071(8)
O8 0.286(11) 0.218(8) 0.121(5) -0.013(5) -0.011(6) -0.071(8)

_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
Ni C8A 1.861(8) . ?
Ni C9A 1.863(8) . ?
Ni C8 1.876(9) . ?
Ni C9 1.880(9) . ?
Cu1 N1 2.010(8) . ?
Cu1 N3 2.020(8) . ?
Cu1 N4A 2.039(7) 2_646 ?
Cu1 N2 2.056(7) . ?
Cu1 N5A 2.204(7) . ?
Cu2 N1A 1.988(8) . ?
Cu2 N3A 2.022(8) . ?
Cu2 N4 2.039(8) . ?
Cu2 N2A 2.073(7) . ?
Cu2 N5 2.163(7) 2_646 ?
N1 C1 1.467(13) . ?
N2 C4 1.504(12) . ?
N2 C3 1.525(11) . ?
N2 C7 1.530(11) . ?
N3 C6 1.449(12) . ?
N4 C8A 1.139(10) . ?
N5 C9 1.159(10) . ?
N5 Cu2 2.163(7) 2_656 ?
N1A C1A 1.464(14) . ?
N2A C4A 1.487(12) . ?
N2A C7A 1.504(12) . ?
N2A C3A 1.526(13) . ?
N3A C6A 1.437(12) . ?
N4A C8 1.126(9) . ?
N4A Cu1 2.039(7) 2_656 ?
N5A C9A 1.152(9) . ?
C1 C2 1.524(14) . ?
C2 C3 1.482(15) . ?
C4 C5 1.525(16) . ?
C5 C6 1.531(16) . ?
C1A C2A 1.529(15) . ?
C2A C3A 1.488(15) . ?
C4A C5A 1.548(15) . ?
C5A C6A 1.492(13) . ?
Cl1 O4 1.306(15) . ?
Cl1 O1B 1.35(2) . ?
Cl1 O1 1.365(14) . ?
Cl1 O4B 1.38(3) . ?
Cl1 O3 1.428(17) . ?
Cl1 O2 1.433(17) . ?
Cl1 O2B 1.45(2) . ?
Cl1 O3B 1.59(3) . ?
O1 O4B 0.94(4) . ?
O1 O3B 1.62(4) . ?
O2 O2B 0.70(3) . ?
O3 O1B 1.19(2) . ?
O4 O3B 1.36(3) . ?
O4 O1B 1.39(2) . ?
Cl2 O8 1.223(17) . ?
Cl2 O6B 1.36(2) . ?
Cl2 O5 1.358(9) . ?
Cl2 O7B 1.43(2) . ?
Cl2 O7 1.452(17) . ?
Cl2 O6 1.470(18) . ?
Cl2 O8B 1.530(19) . ?
O6 O6B 0.51(3) . ?
O7 O7B 1.08(3) . ?
O7 O6B 1.80(3) . ?
O8 O8B 0.80(2) . ?
O8 O7B 1.56(3) . ?

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
C8A Ni C9A 92.1(4) . . ?
C8A Ni C8 88.0(4) . . ?
C9A Ni C8 176.5(4) . . ?
C8A Ni C9 175.8(4) . . ?
C9A Ni C9 88.8(4) . . ?
C8 Ni C9 91.4(3) . . ?
N1 Cu1 N3 162.1(3) . . ?
N1 Cu1 N4A 86.3(3) . 2_646 ?
N3 Cu1 N4A 85.1(3) . 2_646 ?
N1 Cu1 N2 91.0(3) . . ?
N3 Cu1 N2 94.3(3) . . ?
N4A Cu1 N2 168.6(3) 2_646 . ?
N1 Cu1 N5A 102.9(3) . . ?
N3 Cu1 N5A 93.3(3) . . ?
N4A Cu1 N5A 93.8(3) 2_646 . ?
N2 Cu1 N5A 97.6(3) . . ?
N1A Cu2 N3A 163.0(4) . . ?
N1A Cu2 N4 87.0(3) . . ?
N3A Cu2 N4 85.3(3) . . ?
N1A Cu2 N2A 92.5(3) . . ?
N3A Cu2 N2A 91.9(3) . . ?
N4 Cu2 N2A 168.0(3) . . ?
N1A Cu2 N5 97.0(4) . 2_646 ?
N3A Cu2 N5 98.8(3) . 2_646 ?
N4 Cu2 N5 95.2(3) . 2_646 ?
N2A Cu2 N5 96.8(3) . 2_646 ?
C1 N1 Cu1 117.5(6) . . ?
C4 N2 C3 103.9(8) . . ?
C4 N2 C7 110.6(8) . . ?
C3 N2 C7 110.2(8) . . ?
C4 N2 Cu1 113.6(6) . . ?
C3 N2 Cu1 112.0(5) . . ?
C7 N2 Cu1 106.5(5) . . ?
C6 N3 Cu1 121.6(6) . . ?
C8A N4 Cu2 172.4(8) . . ?
C9 N5 Cu2 159.8(7) . 2_656 ?
C1A N1A Cu2 119.5(7) . . ?
C4A N2A C7A 111.3(8) . . ?
C4A N2A C3A 102.3(8) . . ?
C7A N2A C3A 112.5(8) . . ?
C4A N2A Cu2 111.6(6) . . ?
C7A N2A Cu2 108.5(6) . . ?
C3A N2A Cu2 110.6(6) . . ?
C6A N3A Cu2 121.7(6) . . ?
C8 N4A Cu1 173.8(7) . 2_656 ?
C9A N5A Cu1 148.8(7) . . ?
N1 C1 C2 112.0(9) . . ?
C3 C2 C1 115.3(9) . . ?
C2 C3 N2 117.1(9) . . ?
N2 C4 C5 114.3(9) . . ?
C4 C5 C6 110.7(9) . . ?
N3 C6 C5 111.0(9) . . ?
N4A C8 Ni 176.5(8) . . ?
N5 C9 Ni 177.0(8) . . ?
N1A C1A C2A 111.0(9) . . ?
C3A C2A C1A 112.6(10) . . ?
C2A C3A N2A 114.9(10) . . ?
N2A C4A C5A 115.5(9) . . ?
C6A C5A C4A 112.0(8) . . ?
N3A C6A C5A 110.5(9) . . ?
N4 C8A Ni 175.4(9) . . ?
N5A C9A Ni 178.4(7) . . ?
O4 Cl1 O1B 62.8(11) . . ?
O4 Cl1 O1 115.1(9) . . ?
O1B Cl1 O1 118.1(11) . . ?
O4 Cl1 O4B 154.4(19) . . ?
O1B Cl1 O4B 118.4(14) . . ?
O1 Cl1 O4B 39.9(18) . . ?
O4 Cl1 O3 110.8(9) . . ?
O1B Cl1 O3 50.5(9) . . ?
O1 Cl1 O3 110.6(10) . . ?
O4B Cl1 O3 81.7(18) . . ?
O4 Cl1 O2 114.7(10) . . ?
O1B Cl1 O2 133.8(11) . . ?
O1 Cl1 O2 104.7(8) . . ?
O4B Cl1 O2 83.4(16) . . ?
O3 Cl1 O2 99.8(8) . . ?
O4 Cl1 O2B 88.7(12) . . ?
O1B Cl1 O2B 113.7(12) . . ?
O1 Cl1 O2B 128.2(12) . . ?
O4B Cl1 O2B 111.4(14) . . ?
O3 Cl1 O2B 101.1(13) . . ?
O2 Cl1 O2B 28.0(10) . . ?
O4 Cl1 O3B 54.9(13) . . ?
O1B Cl1 O3B 106.2(13) . . ?
O1 Cl1 O3B 65.9(14) . . ?
O4B Cl1 O3B 104.1(14) . . ?
O3 Cl1 O3B 153.5(12) . . ?
O2 Cl1 O3B 106.6(13) . . ?
O2B Cl1 O3B 100.7(11) . . ?
O4B O1 Cl1 71(2) . . ?
O4B O1 O3B 131(3) . . ?
Cl1 O1 O3B 63.6(13) . . ?
O2B O2 Cl1 78(3) . . ?
O1B O3 Cl1 61.4(14) . . ?
Cl1 O4 O3B 73.1(16) . . ?
Cl1 O4 O1B 60.2(12) . . ?
O3B O4 O1B 118(2) . . ?
O3 O1B Cl1 68.1(14) . . ?
O3 O1B O4 122(2) . . ?
Cl1 O1B O4 57.0(11) . . ?
O2 O2B Cl1 74(3) . . ?
O4 O3B Cl1 52.0(13) . . ?
O4 O3B O1 98(2) . . ?
Cl1 O3B O1 50.5(12) . . ?
O1 O4B Cl1 69(2) . . ?
O8 Cl2 O6B 113.3(17) . . ?
O8 Cl2 O5 121.5(9) . . ?
O6B Cl2 O5 117.8(12) . . ?
O8 Cl2 O7B 71.5(12) . . ?
O6B Cl2 O7B 110.7(11) . . ?
O5 Cl2 O7B 112.6(10) . . ?
O8 Cl2 O7 112.3(11) . . ?
O6B Cl2 O7 79.9(12) . . ?
O5 Cl2 O7 103.1(8) . . ?
O7B Cl2 O7 44.0(12) . . ?
O8 Cl2 O6 112.6(11) . . ?
O6B Cl2 O6 20.4(13) . . ?
O5 Cl2 O6 105.8(9) . . ?
O7B Cl2 O6 130.8(14) . . ?
O7 Cl2 O6 98.8(8) . . ?
O8 Cl2 O8B 31.4(11) . . ?
O6B Cl2 O8B 108.1(10) . . ?
O5 Cl2 O8B 103.9(8) . . ?
O7B Cl2 O8B 102.3(12) . . ?
O7 Cl2 O8B 143.5(9) . . ?
O6 Cl2 O8B 96.9(12) . . ?
O6B O6 Cl2 67(3) . . ?
O7B O7 Cl2 67.1(14) . . ?
O7B O7 O6B 102.5(18) . . ?
Cl2 O7 O6B 47.7(9) . . ?
O8B O8 Cl2 96(2) . . ?
O8B O8 O7B 154(3) . . ?
Cl2 O8 O7B 60.5(12) . . ?
O6 O6B Cl2 92(4) . . ?
O6 O6B O7 139(4) . . ?
Cl2 O6B O7 52.4(9) . . ?
O7 O7B Cl2 68.9(17) . . ?
O7 O7B O8 113(2) . . ?
Cl2 O7B O8 47.9(10) . . ?
O8 O8B Cl2 52.7(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Cu1 N1 C1 -158.7(9) . . . . ?
N4A Cu1 N1 C1 139.8(7) 2_646 . . . ?
N2 Cu1 N1 C1 -51.3(7) . . . . ?
N5A Cu1 N1 C1 46.7(7) . . . . ?
N1 Cu1 N2 C4 163.6(7) . . . . ?
N3 Cu1 N2 C4 -33.5(7) . . . . ?
N4A Cu1 N2 C4 -120.0(15) 2_646 . . . ?
N5A Cu1 N2 C4 60.4(7) . . . . ?
N1 Cu1 N2 C3 46.2(7) . . . . ?
N3 Cu1 N2 C3 -150.9(7) . . . . ?
N4A Cu1 N2 C3 122.6(15) 2_646 . . . ?
N5A Cu1 N2 C3 -56.9(7) . . . . ?
N1 Cu1 N2 C7 -74.4(7) . . . . ?
N3 Cu1 N2 C7 88.6(7) . . . . ?
N4A Cu1 N2 C7 2.0(19) 2_646 . . . ?
N5A Cu1 N2 C7 -177.5(7) . . . . ?
N1 Cu1 N3 C6 141.3(10) . . . . ?
N4A Cu1 N3 C6 -157.0(8) 2_646 . . . ?
N2 Cu1 N3 C6 34.4(8) . . . . ?
N5A Cu1 N3 C6 -63.5(8) . . . . ?
N1A Cu2 N4 C8A -11(6) . . . . ?
N3A Cu2 N4 C8A 154(6) . . . . ?
N2A Cu2 N4 C8A 77(6) . . . . ?
N5 Cu2 N4 C8A -107(6) 2_646 . . . ?
N3A Cu2 N1A C1A 150.9(10) . . . . ?
N4 Cu2 N1A C1A -146.1(8) . . . . ?
N2A Cu2 N1A C1A 45.9(8) . . . . ?
N5 Cu2 N1A C1A -51.3(8) 2_646 . . . ?
N1A Cu2 N2A C4A -156.4(7) . . . . ?
N3A Cu2 N2A C4A 40.0(8) . . . . ?
N4 Cu2 N2A C4A 116.3(16) . . . . ?
N5 Cu2 N2A C4A -59.0(7) 2_646 . . . ?
N1A Cu2 N2A C7A 80.7(6) . . . . ?
N3A Cu2 N2A C7A -82.9(6) . . . . ?
N4 Cu2 N2A C7A -6.6(18) . . . . ?
N5 Cu2 N2A C7A 178.0(6) 2_646 . . . ?
N1A Cu2 N2A C3A -43.2(7) . . . . ?
N3A Cu2 N2A C3A 153.2(7) . . . . ?
N4 Cu2 N2A C3A -130.5(14) . . . . ?
N5 Cu2 N2A C3A 54.1(7) 2_646 . . . ?
N1A Cu2 N3A C6A -147.9(10) . . . . ?
N4 Cu2 N3A C6A 148.9(8) . . . . ?
N2A Cu2 N3A C6A -42.8(8) . . . . ?
N5 Cu2 N3A C6A 54.3(8) 2_646 . . . ?
N1 Cu1 N5A C9A 152.6(12) . . . . ?
N3 Cu1 N5A C9A -19.8(12) . . . . ?
N4A Cu1 N5A C9A 65.5(12) 2_646 . . . ?
N2 Cu1 N5A C9A -114.6(12) . . . . ?
Cu1 N1 C1 C2 61.9(11) . . . . ?
N1 C1 C2 C3 -61.0(13) . . . . ?
C1 C2 C3 N2 62.5(13) . . . . ?
C4 N2 C3 C2 177.9(9) . . . . ?
C7 N2 C3 C2 59.3(11) . . . . ?
Cu1 N2 C3 C2 -59.1(10) . . . . ?
C3 N2 C4 C5 -179.9(9) . . . . ?
C7 N2 C4 C5 -61.7(11) . . . . ?
Cu1 N2 C4 C5 58.1(10) . . . . ?
N2 C4 C5 C6 -75.5(12) . . . . ?
Cu1 N3 C6 C5 -54.0(11) . . . . ?
C4 C5 C6 N3 69.6(12) . . . . ?
Cu1 N4A C8 Ni 26(20) 2_656 . . . ?
C8A Ni C8 N4A -57(13) . . . . ?
C9A Ni C8 N4A 35(17) . . . . ?
C9 Ni C8 N4A 127(13) . . . . ?
Cu2 N5 C9 Ni -140(14) 2_656 . . . ?
C8A Ni C9 N5 6(18) . . . . ?
C9A Ni C9 N5 -96(15) . . . . ?
C8 Ni C9 N5 87(15) . . . . ?
Cu2 N1A C1A C2A -59.4(12) . . . . ?
N1A C1A C2A C3A 66.0(14) . . . . ?
C1A C2A C3A N2A -71.7(13) . . . . ?
C4A N2A C3A C2A -178.7(9) . . . . ?
C7A N2A C3A C2A -59.2(11) . . . . ?
Cu2 N2A C3A C2A 62.4(10) . . . . ?
C7A N2A C4A C5A 60.6(11) . . . . ?
C3A N2A C4A C5A -179.1(8) . . . . ?
Cu2 N2A C4A C5A -60.8(10) . . . . ?
N2A C4A C5A C6A 72.9(13) . . . . ?
Cu2 N3A C6A C5A 58.8(11) . . . . ?
C4A C5A C6A N3A -66.2(12) . . . . ?
Cu2 N4 C8A Ni -8(15) . . . . ?
C9A Ni C8A N4 127(10) . . . . ?
C8 Ni C8A N4 -57(10) . . . . ?
C9 Ni C8A N4 25(13) . . . . ?
Cu1 N5A C9A Ni 50(29) . . . . ?
C8A Ni C9A N5A -124(28) . . . . ?
C8 Ni C9A N5A 144(26) . . . . ?
C9 Ni C9A N5A 52(28) . . . . ?
O4 Cl1 O1 O4B 173(2) . . . . ?
O1B Cl1 O1 O4B 102(2) . . . . ?
O3 Cl1 O1 O4B 46(3) . . . . ?
O2 Cl1 O1 O4B -60(3) . . . . ?
O2B Cl1 O1 O4B -77(3) . . . . ?
O3B Cl1 O1 O4B -162(3) . . . . ?
O4 Cl1 O1 O3B -25.0(17) . . . . ?
O1B Cl1 O1 O3B -96.2(15) . . . . ?
O4B Cl1 O1 O3B 162(3) . . . . ?
O3 Cl1 O1 O3B -151.5(13) . . . . ?
O2 Cl1 O1 O3B 101.9(15) . . . . ?
O2B Cl1 O1 O3B 84.7(15) . . . . ?
O4 Cl1 O2 O2B -23(3) . . . . ?
O1B Cl1 O2 O2B 52(3) . . . . ?
O1 Cl1 O2 O2B -150(3) . . . . ?
O4B Cl1 O2 O2B 176(4) . . . . ?
O3 Cl1 O2 O2B 95(3) . . . . ?
O3B Cl1 O2 O2B -82(3) . . . . ?
O4 Cl1 O3 O1B -18.9(16) . . . . ?
O1 Cl1 O3 O1B 110.0(14) . . . . ?
O4B Cl1 O3 O1B 138(2) . . . . ?
O2 Cl1 O3 O1B -140.2(13) . . . . ?
O2B Cl1 O3 O1B -111.7(15) . . . . ?
O3B Cl1 O3 O1B 33(4) . . . . ?
O1B Cl1 O4 O3B 138.2(18) . . . . ?
O1 Cl1 O4 O3B 28(2) . . . . ?
O4B Cl1 O4 O3B 39(4) . . . . ?
O3 Cl1 O4 O3B 154.5(15) . . . . ?
O2 Cl1 O4 O3B -93.5(17) . . . . ?
O2B Cl1 O4 O3B -104.1(14) . . . . ?
O1 Cl1 O4 O1B -110.1(14) . . . . ?
O4B Cl1 O4 O1B -100(4) . . . . ?
O3 Cl1 O4 O1B 16.3(14) . . . . ?
O2 Cl1 O4 O1B 128.3(13) . . . . ?
O2B Cl1 O4 O1B 117.7(14) . . . . ?
O3B Cl1 O4 O1B -138.2(18) . . . . ?
Cl1 O3 O1B O4 19.6(16) . . . . ?
O4 Cl1 O1B O3 160.1(17) . . . . ?
O1 Cl1 O1B O3 -94.4(15) . . . . ?
O4B Cl1 O1B O3 -49(3) . . . . ?
O2 Cl1 O1B O3 61.0(18) . . . . ?
O2B Cl1 O1B O3 84.8(17) . . . . ?
O3B Cl1 O1B O3 -165.3(16) . . . . ?
O1 Cl1 O1B O4 105.5(12) . . . . ?
O4B Cl1 O1B O4 151(2) . . . . ?
O3 Cl1 O1B O4 -160.1(17) . . . . ?
O2 Cl1 O1B O4 -99.1(16) . . . . ?
O2B Cl1 O1B O4 -75.3(15) . . . . ?
O3B Cl1 O1B O4 34.6(17) . . . . ?
Cl1 O4 O1B O3 -21.8(18) . . . . ?
O3B O4 O1B O3 -68(3) . . . . ?
O3B O4 O1B Cl1 -46(2) . . . . ?
O4 Cl1 O2B O2 159(3) . . . . ?
O1B Cl1 O2B O2 -142(3) . . . . ?
O1 Cl1 O2B O2 38(3) . . . . ?
O4B Cl1 O2B O2 -5(4) . . . . ?
O3 Cl1 O2B O2 -90(3) . . . . ?
O3B Cl1 O2B O2 105(3) . . . . ?
O1B O4 O3B Cl1 41.1(17) . . . . ?
Cl1 O4 O3B O1 -21.4(14) . . . . ?
O1B O4 O3B O1 20(3) . . . . ?
O1B Cl1 O3B O4 -38.1(18) . . . . ?
O1 Cl1 O3B O4 -152.1(19) . . . . ?
O4B Cl1 O3B O4 -163.9(17) . . . . ?
O3 Cl1 O3B O4 -64(4) . . . . ?
O2 Cl1 O3B O4 108.9(13) . . . . ?
O2B Cl1 O3B O4 80.7(16) . . . . ?
O4 Cl1 O3B O1 152.1(19) . . . . ?
O1B Cl1 O3B O1 114.0(13) . . . . ?
O4B Cl1 O3B O1 -12(2) . . . . ?
O3 Cl1 O3B O1 88(3) . . . . ?
O2 Cl1 O3B O1 -99.0(11) . . . . ?
O2B Cl1 O3B O1 -127.2(13) . . . . ?
O4B O1 O3B O4 45(5) . . . . ?
Cl1 O1 O3B O4 21.9(14) . . . . ?
O4B O1 O3B Cl1 23(4) . . . . ?
O3B O1 O4B Cl1 -22(4) . . . . ?
O4 Cl1 O4B O1 -15(5) . . . . ?
O1B Cl1 O4B O1 -101(3) . . . . ?
O3 Cl1 O4B O1 -137(2) . . . . ?
O2 Cl1 O4B O1 122(2) . . . . ?
O2B Cl1 O4B O1 125(2) . . . . ?
O3B Cl1 O4B O1 17(3) . . . . ?
O8 Cl2 O6 O6B -96(4) . . . . ?
O5 Cl2 O6 O6B 129(4) . . . . ?
O7B Cl2 O6 O6B -12(5) . . . . ?
O7 Cl2 O6 O6B 22(4) . . . . ?
O8B Cl2 O6 O6B -125(4) . . . . ?
O8 Cl2 O7 O7B -23(2) . . . . ?
O6B Cl2 O7 O7B -134.6(18) . . . . ?
O5 Cl2 O7 O7B 109.0(16) . . . . ?
O6 Cl2 O7 O7B -142.3(17) . . . . ?
O8B Cl2 O7 O7B -28(2) . . . . ?
O8 Cl2 O7 O6B 111.2(18) . . . . ?
O5 Cl2 O7 O6B -116.4(12) . . . . ?
O7B Cl2 O7 O6B 134.6(18) . . . . ?
O6 Cl2 O7 O6B -7.7(15) . . . . ?
O8B Cl2 O7 O6B 106.8(16) . . . . ?
O6B Cl2 O8 O8B -87(2) . . . . ?
O5 Cl2 O8 O8B 62(3) . . . . ?
O7B Cl2 O8 O8B 168(3) . . . . ?
O7 Cl2 O8 O8B -175(2) . . . . ?
O6 Cl2 O8 O8B -65(3) . . . . ?
O6B Cl2 O8 O7B 105.2(14) . . . . ?
O5 Cl2 O8 O7B -105.7(13) . . . . ?
O7 Cl2 O8 O7B 16.9(16) . . . . ?
O6 Cl2 O8 O7B 127.4(15) . . . . ?
O8B Cl2 O8 O7B -168(3) . . . . ?
Cl2 O6 O6B O7 -27(5) . . . . ?
O8 Cl2 O6B O6 92(4) . . . . ?
O5 Cl2 O6B O6 -58(5) . . . . ?
O7B Cl2 O6B O6 170(4) . . . . ?
O7 Cl2 O6B O6 -158(4) . . . . ?
O8B Cl2 O6B O6 59(5) . . . . ?
O8 Cl2 O6B O7 -110.1(12) . . . . ?
O5 Cl2 O6B O7 99.6(10) . . . . ?
O7B Cl2 O6B O7 -31.9(14) . . . . ?
O6 Cl2 O6B O7 158(4) . . . . ?
O8B Cl2 O6B O7 -143.2(9) . . . . ?
O7B O7 O6B O6 78(7) . . . . ?
Cl2 O7 O6B O6 36(7) . . . . ?
O7B O7 O6B Cl2 42.2(18) . . . . ?
O6B O7 O7B Cl2 -32.7(13) . . . . ?
Cl2 O7 O7B O8 18.2(15) . . . . ?
O6B O7 O7B O8 -14(3) . . . . ?
O8 Cl2 O7B O7 157(2) . . . . ?
O6B Cl2 O7B O7 49(2) . . . . ?
O5 Cl2 O7B O7 -85.6(17) . . . . ?
O6 Cl2 O7B O7 53(2) . . . . ?
O8B Cl2 O7B O7 163.5(14) . . . . ?
O6B Cl2 O7B O8 -108.7(18) . . . . ?
O5 Cl2 O7B O8 117.2(11) . . . . ?
O7 Cl2 O7B O8 -157(2) . . . . ?
O6 Cl2 O7B O8 -104.3(15) . . . . ?
O8B Cl2 O7B O8 6.3(15) . . . . ?
O8B O8 O7B O7 -51(8) . . . . ?
Cl2 O8 O7B O7 -23(2) . . . . ?
O8B O8 O7B Cl2 -28(7) . . . . ?
O7B O8 O8B Cl2 24(6) . . . . ?
O6B Cl2 O8B O8 105(3) . . . . ?
O5 Cl2 O8B O8 -129(2) . . . . ?
O7B Cl2 O8B O8 -12(3) . . . . ?
O7 Cl2 O8B O8 8(3) . . . . ?
O6 Cl2 O8B O8 123(2) . . . . ?

_diffrn_measured_fraction_theta_max    0.983
_diffrn_reflns_theta_full              23.96
_diffrn_measured_fraction_theta_full   0.983
_refine_diff_density_max    0.826
_refine_diff_density_min   -0.678
_refine_diff_density_rms    0.093