# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1281

data_global
# 1. SUBMISSION DETAILS

_publ_contact_autor
;
        Michael J. Zaworotko
        Department of Chemistry
        The University of Winnipeg
        Winnipeg
        Manitoba, R3B 2E9
        Canada
;
_publ_contact_author_phone        '+ 204 786-9764'
_publ_contact_author_fax          '+ 204 783-7981'
_publ_contact_author_email        'mike.zaworotko@uwinnipeg.ca'
_publ_requested_journal           
'Journal of Chemical Society, Chemical Communications'
_publ_requested_coeditor_name     ?

_publ_contact_letter
;
  ?
;

#==============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title
;
 Covalent and Noncovalent Interpenetrating Planar Networks in the Crystal
 Structure of {[Ni(4,4'-bipyridine)~2~(NO~3~)~2~]*2Pyrene}~n~
;

loop_
 _publ_author_name
 _publ_author_address
     'Biradha, Kumar'
;    Department of Chemistry
      The University of Winnipeg
      Winnipeg
      Manitoba, R3B 2E9
      Canada
;
     'Domasevitch, Konstantin V.'
;    Department of Chemistry
      The University of Winnipeg
      Winnipeg
      Manitoba, R3B 2E9
      Canada
;
     'Moulton, Brian'
;    Department of Chemistry
      The University of Winnipeg
      Winnipeg
      Manitoba, R3B 2E9
      Canada
;
     'Seward, Corey'
;    Department of Chemistry
      The University of Winnipeg
      Winnipeg
      Manitoba, R3B 2E9
      Canada
;
     'Zaworotko, Michael J.'
;    Department of Chemistry
      The University of Winnipeg
      Winnipeg
      Manitoba, R3B 2E9
      Canada
;

#==============================================================================

# 4. TEXT

_publ_section_abstract
;

;
_publ_section_comment
;
 The crystal structure of {[Ni(4,4'-bipyridine)~2~(NO~3~)~2~]*2Pyrene}~n~
 reveals the first example of interpenetrating covalent and noncovalent
 2D networks.
;
_publ_section_experimental
;
 The compound was synthesized reacting nickel(II) nitrate with
 4,4'-bipyridine and pyrene in methanol solution
;
_publ_section_references
;

;

_publ_section_figure_captions
;

;
_publ_section_acknowledgements
;
 We acknowledge the generous financial support of the N.S.E.R.C (Canada)
 in the form of a research grant (M.J.Z.).
;

#==============================================================================

data_cs057 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 bis(4,4'-bipyridine)dinitratonickel(II) 1:2 complex with pyrene
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C52 H36 N6 Ni O6' 
_chemical_formula_weight          899.58 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    Pn 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y, z+1/2' 
 
_cell_length_a                    11.3602(6) 
_cell_length_b                    22.7707(13) 
_cell_length_c                    15.8580(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.9560(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      4092.4(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.460 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1864 
_exptl_absorpt_coefficient_mu     0.538 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_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        'SMART CCD Siemens' 
_diffrn_measurement_method        'thetha scans' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             20321 
_diffrn_reflns_av_R_equivalents   0.0236 
_diffrn_reflns_av_sigmaI/netI     0.0509 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        30 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          0.89 
_diffrn_reflns_theta_max          27.95 
_reflns_number_total              15136 
_reflns_number_observed           10600 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         'SAINT Siemens' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Cerius2, v.3.8' 
_computing_publication_material   'SHELXL-92' 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 859 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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            fullcycle 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] 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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.48(2) 
_refine_ls_number_reflns          14277 
_refine_ls_number_parameters      1172 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0651 
_refine_ls_R_factor_obs           0.0409 
_refine_ls_wR_factor_all          0.1250 
_refine_ls_wR_factor_obs          0.1031 
_refine_ls_goodness_of_fit_all    1.017 
_refine_ls_goodness_of_fit_obs    1.114 
_refine_ls_restrained_S_all       1.124 
_refine_ls_restrained_S_obs       1.114 
_refine_ls_shift/esd_max          0.008 
_refine_ls_shift/esd_mean         0.001 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ni1 Ni 0.84513(11) 0.48775(3) 0.09083(9) 0.0138(2) Uani 1 d . . 
Ni2 Ni 0.85898(11) -0.01216(3) 0.08234(9) 0.0152(2) Uani 1 d . . 
O1 O 0.8143(5) 0.4944(2) -0.0416(3) 0.0281(11) Uani 1 d . . 
O2 O 0.8624(5) 0.5347(3) -0.1545(4) 0.067(2) Uani 1 d . . 
O3 O 0.9462(6) 0.4581(3) -0.1152(5) 0.100(2) Uani 1 d . . 
O4 O 0.8433(4) 0.4792(2) 0.2218(3) 0.0271(11) Uani 1 d . . 
O5 O 0.7963(5) 0.5139(3) 0.3416(4) 0.073(2) Uani 1 d . . 
O6 O 0.9768(4) 0.5164(2) 0.3115(3) 0.0291(10) Uani 1 d . . 
O7 O 0.8896(4) -0.0057(2) 0.2119(3) 0.0236(10) Uani 1 d . . 
O8 O 0.7519(4) -0.0422(2) 0.2849(3) 0.0419(12) Uani 1 d . . 
O9 O 0.8629(7) 0.0263(4) 0.3355(4) 0.113(3) Uani 1 d . . 
O10 O 0.8548(4) -0.0207(2) -0.0503(3) 0.0358(13) Uani 1 d . . 
O11 O 0.9052(5) 0.0213(3) -0.1628(3) 0.073(2) Uani 1 d . . 
O12 O 0.7279(6) 0.0180(3) -0.1367(4) 0.082(2) Uani 1 d . . 
N1 N 0.8492(4) -0.4184(2) 0.0967(3) 0.0131(10) Uani 1 d . . 
N2 N 0.8591(4) -0.1065(2) 0.0863(3) 0.0177(11) Uani 1 d . . 
N3 N 0.8630(5) 0.0811(2) 0.0807(4) 0.0216(12) Uani 1 d . . 
N4 N 0.8477(4) 0.3940(2) 0.0895(3) 0.0167(11) Uani 1 d . . 
N5 N 1.0323(4) 0.4910(2) 0.0938(4) 0.0159(12) Uani 1 d . . 
N6 N 1.6572(4) 0.4895(2) 0.0911(3) 0.0133(11) Uani 1 d . . 
N7 N 0.6749(5) -0.0094(2) 0.0817(4) 0.0193(12) Uani 1 d . . 
N8 N 0.0482(5) -0.0096(2) 0.0840(4) 0.0199(13) Uani 1 d . . 
N9 N 0.8761(5) 0.4929(2) -0.1058(4) 0.0208(11) Uani 1 d . . 
N10 N 0.8743(4) 0.5063(2) 0.2926(4) 0.0183(10) Uani 1 d . . 
N11 N 0.8396(6) -0.0022(3) 0.2799(4) 0.037(2) Uani 1 d . . 
N12 N 0.8442(7) 0.0010(3) -0.1165(4) 0.048(2) Uani 1 d . . 
C1 C 0.9104(6) -0.3891(3) 0.1520(4) 0.0231(15) Uani 1 d . . 
H1A H 0.9534(6) -0.4094(3) 0.1947(4) 0.028 Uiso 1 calc R . 
C2 C 0.9163(6) -0.3281(3) 0.1516(4) 0.0256(15) Uani 1 d . . 
H2A H 0.9664(6) -0.3093(3) 0.1919(4) 0.031 Uiso 1 calc R . 
C3 C 0.8518(5) -0.2954(2) 0.0949(4) 0.0155(13) Uani 1 d . . 
C4 C 0.7816(5) -0.3276(3) 0.0305(4) 0.0250(15) Uani 1 d . . 
H4A H 0.7396(5) -0.3079(3) -0.0133(4) 0.030 Uiso 1 calc R . 
C5 C 0.7787(6) -0.3876(3) 0.0359(4) 0.0232(15) Uani 1 d . . 
H5A H 0.7285(6) -0.4085(3) -0.0020(4) 0.028 Uiso 1 calc R . 
C6 C 0.8500(6) -0.2308(3) 0.0903(5) 0.0207(14) Uani 1 d . . 
C7 C 0.8682(5) -0.1960(2) 0.1651(4) 0.0214(14) Uani 1 d . . 
H7A H 0.8794(5) -0.2134(2) 0.2181(4) 0.026 Uiso 1 calc R . 
C8 C 0.8684(6) -0.1356(3) 0.1561(4) 0.0243(15) Uani 1 d . . 
H8A H 0.8762(6) -0.1136(3) 0.2056(4) 0.029 Uiso 1 calc R . 
C9 C 0.8407(6) -0.2005(2) 0.0166(4) 0.0248(15) Uani 1 d . . 
H9A H 0.8306(6) -0.2215(2) -0.0337(4) 0.030 Uiso 1 calc R . 
C10 C 0.8455(6) -0.1397(3) 0.0126(4) 0.0248(15) Uani 1 d . . 
H10A H 0.8397(6) -0.1210(3) -0.0397(4) 0.030 Uiso 1 calc R . 
C11 C 0.9212(6) 0.1120(3) 0.1364(4) 0.029(2) Uani 1 d . . 
H11A H 0.9654(6) 0.0921(3) 0.1790(4) 0.034 Uiso 1 calc R . 
C12 C 0.9237(6) 0.1731(3) 0.1382(4) 0.026(2) Uani 1 d . . 
H12A H 0.9729(6) 0.1920(3) 0.1790(4) 0.032 Uiso 1 calc R . 
C13 C 0.8580(6) 0.2050(3) 0.0837(4) 0.0237(15) Uani 1 d . . 
C14 C 0.7914(6) 0.1738(3) 0.0171(4) 0.0222(14) Uani 1 d . . 
H14A H 0.7490(6) 0.1936(3) -0.0264(4) 0.027 Uiso 1 calc R . 
C15 C 0.7932(6) 0.1141(3) 0.0205(4) 0.0242(15) Uani 1 d . . 
H15A H 0.7455(6) 0.0936(3) -0.0195(4) 0.029 Uiso 1 calc R . 
C16 C 0.8502(6) 0.2707(2) 0.0825(4) 0.0174(13) Uani 1 d . . 
C17 C 0.8391(6) 0.3027(3) 0.0117(4) 0.030(2) Uani 1 d . . 
H17A H 0.8330(6) 0.2834(3) -0.0401(4) 0.036 Uiso 1 calc R . 
C18 C 0.8364(6) 0.3637(3) 0.0127(4) 0.0233(15) Uani 1 d . . 
H18A H 0.8270(6) 0.3844(3) -0.0379(4) 0.028 Uiso 1 calc R . 
C19 C 0.8640(6) 0.3017(3) 0.1604(4) 0.028(2) Uani 1 d . . 
H19A H 0.8752(6) 0.2819(3) 0.2117(4) 0.034 Uiso 1 calc R . 
C20 C 0.8602(6) 0.3616(2) 0.1570(4) 0.024(2) Uani 1 d . . 
H20A H 0.8674(6) 0.3813(2) 0.2084(4) 0.029 Uiso 1 calc R . 
C21 C 1.0871(6) 0.5200(3) 0.0313(5) 0.030(2) Uani 1 d . . 
H21A H 1.0400(6) 0.5391(3) -0.0105(5) 0.036 Uiso 1 calc R . 
C22 C 1.2065(6) 0.5226(3) 0.0269(4) 0.025(2) Uani 1 d . . 
H22A H 1.2397(6) 0.5414(3) -0.0178(4) 0.030 Uiso 1 calc R . 
C23 C 1.2784(6) 0.4957(3) 0.0925(4) 0.0207(15) Uani 1 d . . 
C24 C 1.2210(6) 0.4655(3) 0.1567(5) 0.029(2) Uani 1 d . . 
H24A H 1.2643(6) 0.4465(3) 0.2004(5) 0.035 Uiso 1 calc R . 
C25 C 1.0964(5) 0.4653(3) 0.1522(4) 0.0197(13) Uani 1 d . . 
H25A H 1.0589(5) 0.4454(3) 0.1940(4) 0.024 Uiso 1 calc R . 
C26 C 1.4120(5) 0.4946(2) 0.0929(4) 0.0170(14) Uani 1 d . . 
C27 C 1.4653(6) 0.4762(3) 0.0208(4) 0.024(2) Uani 1 d . . 
H27A H 1.4190(6) 0.4654(3) -0.0274(4) 0.029 Uiso 1 calc R . 
C28 C 1.5831(6) 0.4740(3) 0.0209(4) 0.026(2) Uani 1 d . . 
H28A H 1.6168(6) 0.4616(3) -0.0279(4) 0.031 Uiso 1 calc R . 
C29 C 1.4802(6) 0.5103(3) 0.1595(5) 0.025(2) Uani 1 d . . 
H29A H 1.4461(6) 0.5223(3) 0.2083(5) 0.029 Uiso 1 calc R . 
C30 C 1.6035(5) 0.5091(2) 0.1582(4) 0.0170(13) Uani 1 d . . 
H30A H 1.6493(5) 0.5222(2) 0.2053(4) 0.020 Uiso 1 calc R . 
C31 C 0.6000(6) -0.0352(3) 0.0190(5) 0.033(2) Uani 1 d . . 
H31A H 0.6333(6) -0.0556(3) -0.0243(5) 0.039 Uiso 1 calc R . 
C32 C 0.4819(6) -0.0320(3) 0.0183(5) 0.027(2) Uani 1 d . . 
H32A H 0.4365(6) -0.0480(3) -0.0271(5) 0.032 Uiso 1 calc R . 
C33 C 0.4266(5) -0.0060(3) 0.0818(5) 0.0172(14) Uani 1 d . . 
C34 C 0.1163(5) -0.0250(3) 0.1482(4) 0.0223(14) Uani 1 d . . 
H34A H 0.0809(5) -0.0383(3) 0.1958(4) 0.027 Uiso 1 calc R . 
C35 C 0.2424(6) -0.0232(3) 0.1523(5) 0.026(2) Uani 1 d . . 
H35A H 0.2861(6) -0.0338(3) 0.2017(5) 0.032 Uiso 1 calc R . 
C36 C 0.2988(6) -0.0054(3) 0.0820(4) 0.0211(15) Uani 1 d . . 
C37 C 0.2223(6) 0.0117(3) 0.0081(4) 0.0235(15) Uani 1 d . . 
H37A H 0.2534(6) 0.0244(3) -0.0415(4) 0.028 Uiso 1 calc R . 
C38 C 0.1022(6) 0.0080(3) 0.0148(5) 0.031(2) Uani 1 d . . 
H38A H 0.0539(6) 0.0187(3) -0.0324(5) 0.037 Uiso 1 calc R . 
C39 C 0.4980(6) 0.0210(3) 0.1414(5) 0.029(2) Uani 1 d . . 
H39A H 0.4648(6) 0.0414(3) 0.1847(5) 0.035 Uiso 1 calc R . 
C40 C 0.6208(6) 0.0191(3) 0.1392(4) 0.0229(14) Uani 1 d . . 
H40A H 0.6663(6) 0.0391(3) 0.1808(4) 0.028 Uiso 1 calc R . 
C101 C 0.4755(8) 0.2380(4) 0.9013(6) 0.046(2) Uani 1 d . . 
C102 C 0.4424(7) 0.2984(4) 0.9198(5) 0.046(2) Uani 1 d . . 
H10B H 0.3810(7) 0.3063(4) 0.9540(5) 0.055 Uiso 1 calc R . 
C103 C 0.5007(8) 0.3407(4) 0.8874(6) 0.061(3) Uani 1 d . . 
H10C H 0.4751(8) 0.3789(4) 0.8957(6) 0.073 Uiso 1 calc R . 
C104 C 0.6026(7) 0.3324(3) 0.8393(5) 0.032(2) Uani 1 d . . 
C105 C 0.6650(8) 0.3800(4) 0.8015(6) 0.058(3) Uani 1 d . . 
H10D H 0.6423(8) 0.4189(4) 0.8084(6) 0.069 Uiso 1 calc R . 
C106 C 0.7631(8) 0.3653(4) 0.7530(6) 0.056(2) Uani 1 d . . 
H10E H 0.8090(8) 0.3953(4) 0.7329(6) 0.067 Uiso 1 calc R . 
C107 C 0.7903(7) 0.3098(4) 0.7361(5) 0.051(2) Uani 1 d . . 
H10F H 0.8515(7) 0.3026(4) 0.7014(5) 0.061 Uiso 1 calc R . 
C108 C 0.7310(7) 0.2628(4) 0.7679(6) 0.039(2) Uani 1 d . . 
C109 C 0.7621(8) 0.2030(5) 0.7568(6) 0.061(3) Uani 1 d . . 
H10G H 0.8271(8) 0.1948(5) 0.7262(6) 0.073 Uiso 1 calc R . 
C110 C 0.7016(7) 0.1567(3) 0.7886(5) 0.040(2) Uani 1 d . . 
H11B H 0.7237(7) 0.1184(3) 0.7770(5) 0.048 Uiso 1 calc R . 
C111 C 0.6037(8) 0.1672(4) 0.8401(6) 0.044(2) Uani 1 d . . 
C112 C 0.5361(9) 0.1233(4) 0.8697(6) 0.052(2) Uani 1 d . . 
H11C H 0.5512(9) 0.0846(4) 0.8548(6) 0.063 Uiso 1 calc R . 
C113 C 0.4502(9) 0.1343(6) 0.9187(7) 0.081(4) Uani 1 d . . 
H11D H 0.4122(9) 0.1032(6) 0.9435(7) 0.097 Uiso 1 calc R . 
C114 C 0.4147(8) 0.1926(5) 0.9343(7) 0.079(3) Uani 1 d . . 
H11E H 0.3509(8) 0.1999(5) 0.9665(7) 0.095 Uiso 1 calc R . 
C115 C 0.6347(6) 0.2732(3) 0.8201(5) 0.029(2) Uani 1 d . . 
C116 C 0.5716(7) 0.2256(4) 0.8535(5) 0.033(2) Uani 1 d . . 
C201 C 0.6339(7) 0.2361(4) 0.5300(6) 0.046(2) Uani 1 d . . 
H20B H 0.6343(7) 0.2558(4) 0.5814(6) 0.055 Uiso 1 calc R . 
C202 C 0.6523(7) 0.1787(4) 0.5308(6) 0.053(2) Uani 1 d . . 
H20C H 0.6714(7) 0.1602(4) 0.5822(6) 0.064 Uiso 1 calc R . 
C203 C 0.6442(7) 0.1452(4) 0.4577(6) 0.046(2) Uani 1 d . . 
H20D H 0.6541(7) 0.1047(4) 0.4601(6) 0.055 Uiso 1 calc R . 
C204 C 0.6209(7) 0.1734(3) 0.3810(5) 0.036(2) Uani 1 d . . 
C205 C 0.6185(7) 0.1429(4) 0.3003(6) 0.048(2) Uani 1 d . . 
H20E H 0.6304(7) 0.1025(4) 0.3013(6) 0.058 Uiso 1 calc R . 
C206 C 0.6010(6) 0.1681(3) 0.2267(6) 0.037(2) Uani 1 d . . 
H20F H 0.5961(6) 0.1454(3) 0.1779(6) 0.045 Uiso 1 calc R . 
C207 C 0.5885(7) 0.2342(3) 0.2206(6) 0.035(2) Uani 1 d . . 
C208 C 0.5651(8) 0.2607(3) 0.1447(6) 0.045(2) Uani 1 d . . 
H20G H 0.5572(8) 0.2386(3) 0.0953(6) 0.054 Uiso 1 calc R . 
C209 C 0.5527(7) 0.3233(4) 0.1419(6) 0.051(2) Uani 1 d . . 
H20H H 0.5426(7) 0.3429(4) 0.0905(6) 0.062 Uiso 1 calc R . 
C210 C 0.5560(7) 0.3537(3) 0.2166(6) 0.048(2) Uani 1 d . . 
H21B H 0.5466(7) 0.3942(3) 0.2146(6) 0.058 Uiso 1 calc R . 
C211 C 0.5732(7) 0.3263(3) 0.2971(5) 0.033(2) Uani 1 d . . 
C212 C 0.5767(7) 0.3587(3) 0.3747(6) 0.040(2) Uani 1 d . . 
H21C H 0.5689(7) 0.3993(3) 0.3747(6) 0.048 Uiso 1 calc R . 
C213 C 0.5920(7) 0.3276(4) 0.4497(5) 0.045(2) Uani 1 d . . 
H21D H 0.5871(7) 0.3481(4) 0.5000(5) 0.054 Uiso 1 calc R . 
C214 C 0.6135(7) 0.2695(3) 0.4540(5) 0.035(2) Uani 1 d . . 
C215 C 0.6103(6) 0.2340(3) 0.3772(5) 0.027(2) Uani 1 d . . 
C216 C 0.5934(7) 0.2640(3) 0.2984(6) 0.036(2) Uani 1 d . . 
C301 C 0.2789(7) 0.1735(5) 0.2493(6) 0.062(3) Uani 1 d . . 
H30B H 0.3455(7) 0.1744(5) 0.2183(6) 0.075 Uiso 1 calc R . 
C302 C 0.2272(7) 0.1199(3) 0.2664(5) 0.055(2) Uani 1 d . . 
H30C H 0.2614(7) 0.0857(3) 0.2475(5) 0.066 Uiso 1 calc R . 
C303 C 0.1245(7) 0.1157(2) 0.3114(4) 0.035(2) Uani 1 d . . 
H30D H 0.0909(7) 0.0794(2) 0.3221(4) 0.042 Uiso 1 calc R . 
C304 C 0.0737(6) 0.1691(3) 0.3401(4) 0.033(2) Uani 1 d . . 
C305 C -0.0369(7) 0.1713(3) 0.3831(6) 0.045(2) Uani 1 d . . 
H30E H -0.0778(7) 0.1367(3) 0.3924(6) 0.054 Uiso 1 calc R . 
C306 C -0.0786(8) 0.2223(4) 0.4087(5) 0.052(2) Uani 1 d . . 
H30F H -0.1472(8) 0.2217(4) 0.4374(5) 0.063 Uiso 1 calc R . 
C307 C -0.0261(8) 0.2774(4) 0.3953(5) 0.045(2) Uani 1 d . . 
C308 C -0.0720(8) 0.3314(3) 0.4190(5) 0.046(2) Uani 1 d . . 
H30G H -0.1407(8) 0.3330(3) 0.4477(5) 0.055 Uiso 1 calc R . 
C309 C -0.0145(8) 0.3820(4) 0.3995(5) 0.052(2) Uani 1 d . . 
H30H H -0.0449(8) 0.4182(4) 0.4147(5) 0.063 Uiso 1 calc R . 
C310 C 0.0854(9) 0.3800(4) 0.3586(6) 0.069(3) Uani 1 d . . 
H31B H 0.1224(9) 0.4154(4) 0.3475(6) 0.082 Uiso 1 calc R . 
C311 C 0.1339(7) 0.3312(3) 0.3333(5) 0.044(2) Uani 1 d . . 
C312 C 0.2366(8) 0.3314(4) 0.2889(5) 0.043(2) Uani 1 d . . 
H31C H 0.2732(8) 0.3670(4) 0.2786(5) 0.051 Uiso 1 calc R . 
C313 C 0.2828(7) 0.2820(4) 0.2614(5) 0.051(2) Uani 1 d . . 
H31D H 0.3496(7) 0.2838(4) 0.2307(5) 0.061 Uiso 1 calc R . 
C314 C 0.2323(6) 0.2263(4) 0.2779(5) 0.039(2) Uani 1 d . . 
C315 C 0.1278(6) 0.2240(3) 0.3227(4) 0.026(2) Uani 1 d . . 
C316 C 0.0775(7) 0.2768(4) 0.3504(5) 0.036(2) Uani 1 d . . 
C401 C 0.1343(7) 0.2586(4) 1.0289(6) 0.040(2) Uani 1 d . . 
H40B H 0.1343(7) 0.2374(4) 1.0790(6) 0.049 Uiso 1 calc R . 
C402 C 0.1518(7) 0.3156(4) 1.0333(5) 0.044(2) Uani 1 d . . 
H40C H 0.1713(7) 0.3326(4) 1.0858(5) 0.053 Uiso 1 calc R . 
C403 C 0.1416(7) 0.3527(3) 0.9592(6) 0.044(2) Uani 1 d . . 
H40D H 0.1490(7) 0.3933(3) 0.9629(6) 0.052 Uiso 1 calc R . 
C404 C 0.1208(7) 0.3253(4) 0.8848(5) 0.036(2) Uani 1 d . . 
C405 C 0.1177(7) 0.3584(3) 0.8029(6) 0.046(2) Uani 1 d . . 
H40E H 0.1301(7) 0.3988(3) 0.8050(6) 0.055 Uiso 1 calc R . 
C406 C 0.0985(6) 0.3338(3) 0.7288(5) 0.033(2) Uani 1 d . . 
H40F H 0.0922(6) 0.3574(3) 0.6808(5) 0.039 Uiso 1 calc R . 
C407 C 0.0864(6) 0.2681(3) 0.7189(5) 0.031(2) Uani 1 d . . 
C408 C 0.0604(8) 0.2415(4) 0.6430(6) 0.041(2) Uani 1 d . . 
H40G H 0.0491(8) 0.2639(4) 0.5940(6) 0.049 Uiso 1 calc R . 
C409 C 0.0503(7) 0.1786(3) 0.6389(6) 0.044(2) Uani 1 d . . 
H40H H 0.0397(7) 0.1596(3) 0.5871(6) 0.053 Uiso 1 calc R . 
C410 C 0.0566(7) 0.1478(3) 0.7118(5) 0.039(2) Uani 1 d . . 
H41A H 0.0480(7) 0.1072(3) 0.7082(5) 0.047 Uiso 1 calc R . 
C411 C 0.0755(6) 0.1730(3) 0.7941(5) 0.029(2) Uani 1 d . . 
C412 C 0.0827(6) 0.1405(3) 0.8682(5) 0.037(2) Uani 1 d . . 
H41B H 0.0783(6) 0.0998(3) 0.8662(5) 0.044 Uiso 1 calc R . 
C413 C 0.0964(7) 0.1692(4) 0.9455(5) 0.043(2) Uani 1 d . . 
H41C H 0.0925(7) 0.1476(4) 0.9949(5) 0.051 Uiso 1 calc R . 
C414 C 0.1154(7) 0.2278(3) 0.9509(5) 0.034(2) Uani 1 d . . 
C415 C 0.0930(7) 0.2367(3) 0.7984(6) 0.030(2) Uani 1 d . . 
C416 C 0.1110(6) 0.2649(3) 0.8785(5) 0.030(2) Uani 1 d . . 
 
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 
Ni1 0.0102(4) 0.0129(3) 0.0188(5) -0.0021(3) 0.0040(3) 0.0001(3) 
Ni2 0.0125(5) 0.0141(3) 0.0184(5) -0.0017(3) -0.0027(4) -0.0001(3) 
O1 0.029(3) 0.037(3) 0.019(3) 0.001(2) 0.007(2) -0.006(2) 
O2 0.085(3) 0.065(3) 0.058(3) 0.041(3) 0.039(3) 0.011(3) 
O3 0.117(5) 0.074(4) 0.119(5) 0.019(4) 0.083(4) 0.051(4) 
O4 0.036(3) 0.028(2) 0.017(2) 0.005(2) -0.004(2) -0.007(2) 
O5 0.042(3) 0.147(5) 0.034(3) 0.006(3) 0.019(2) 0.019(3) 
O6 0.025(2) 0.026(2) 0.037(3) -0.008(2) 0.000(2) -0.007(2) 
O7 0.016(3) 0.032(3) 0.023(3) -0.002(2) 0.003(2) -0.001(2) 
O8 0.027(2) 0.051(3) 0.047(3) 0.009(2) 0.006(2) -0.010(2) 
O9 0.146(6) 0.160(6) 0.037(3) -0.056(4) 0.028(3) -0.097(5) 
O10 0.055(3) 0.034(3) 0.018(2) 0.015(2) -0.002(2) -0.023(2) 
O11 0.072(4) 0.109(4) 0.035(3) 0.053(3) -0.017(2) -0.060(3) 
O12 0.080(5) 0.100(5) 0.062(5) -0.014(3) -0.021(4) 0.026(4) 
N1 0.012(2) 0.011(2) 0.015(3) 0.005(2) -0.002(2) 0.001(2) 
N2 0.012(3) 0.022(2) 0.019(3) -0.015(2) -0.001(2) 0.002(2) 
N3 0.014(3) 0.022(3) 0.028(3) 0.006(2) -0.004(2) 0.003(2) 
N4 0.020(3) 0.011(2) 0.019(3) -0.013(2) 0.003(2) 0.003(2) 
N5 0.008(3) 0.023(3) 0.017(3) 0.003(2) 0.004(2) -0.004(2) 
N6 0.008(3) 0.019(3) 0.013(3) 0.001(2) 0.000(2) -0.006(2) 
N7 0.016(3) 0.012(2) 0.029(3) -0.001(2) -0.004(2) -0.006(2) 
N8 0.021(3) 0.012(2) 0.027(3) 0.005(2) 0.002(2) -0.008(2) 
N9 0.019(2) 0.021(2) 0.022(3) -0.009(2) 0.002(2) 0.014(2) 
N10 0.009(2) 0.023(2) 0.022(3) -0.005(2) -0.007(2) -0.005(2) 
N11 0.048(4) 0.036(3) 0.027(3) -0.004(2) 0.013(3) 0.021(3) 
N12 0.084(5) 0.038(3) 0.022(3) -0.007(2) 0.001(3) -0.033(3) 
C1 0.031(4) 0.007(3) 0.031(4) 0.007(2) 0.000(3) 0.005(2) 
C2 0.024(4) 0.030(3) 0.021(3) -0.003(3) -0.005(3) -0.006(3) 
C3 0.023(3) 0.004(2) 0.019(3) -0.006(2) -0.001(3) -0.008(2) 
C4 0.017(3) 0.025(3) 0.031(3) -0.015(3) -0.016(3) 0.002(2) 
C5 0.027(4) 0.010(3) 0.030(4) -0.003(2) -0.016(3) 0.006(2) 
C6 0.013(3) 0.025(3) 0.023(3) -0.012(2) 0.000(3) 0.003(2) 
C7 0.031(4) 0.018(3) 0.013(3) -0.005(2) -0.009(2) 0.012(2) 
C8 0.028(4) 0.019(3) 0.026(4) -0.009(3) -0.003(3) 0.004(3) 
C9 0.035(4) 0.005(2) 0.034(3) -0.013(2) 0.003(3) 0.007(2) 
C10 0.028(4) 0.033(3) 0.014(3) -0.001(2) 0.004(3) -0.004(3) 
C11 0.023(4) 0.035(4) 0.027(4) 0.005(3) -0.004(3) 0.002(3) 
C12 0.040(4) 0.015(3) 0.024(3) -0.013(2) -0.005(3) -0.004(3) 
C13 0.018(3) 0.034(3) 0.019(3) -0.007(3) -0.004(3) -0.011(3) 
C14 0.034(4) 0.010(3) 0.021(3) -0.003(2) -0.010(3) 0.003(2) 
C15 0.024(4) 0.030(3) 0.016(3) -0.002(2) -0.014(3) 0.008(3) 
C16 0.019(3) 0.009(2) 0.023(3) -0.012(2) -0.007(2) 0.004(2) 
C17 0.040(4) 0.023(3) 0.026(4) -0.013(3) -0.001(3) 0.018(3) 
C18 0.039(4) 0.019(3) 0.012(3) -0.005(2) -0.002(3) 0.006(3) 
C19 0.040(4) 0.037(3) 0.006(3) -0.009(2) -0.010(2) 0.007(3) 
C20 0.045(4) 0.007(3) 0.021(3) -0.005(2) -0.004(3) -0.005(3) 
C21 0.025(4) 0.036(4) 0.030(4) 0.012(3) 0.009(3) -0.006(3) 
C22 0.027(4) 0.025(3) 0.022(3) 0.013(2) -0.002(3) 0.008(3) 
C23 0.028(4) 0.014(3) 0.020(4) -0.004(2) -0.003(3) -0.001(3) 
C24 0.027(4) 0.037(4) 0.023(4) 0.019(3) -0.001(3) -0.002(3) 
C25 0.005(3) 0.024(3) 0.030(3) 0.002(3) 0.007(2) -0.004(2) 
C26 0.000(3) 0.018(3) 0.035(4) 0.003(2) 0.013(2) 0.002(2) 
C27 0.015(3) 0.043(4) 0.013(3) -0.008(3) -0.002(3) 0.004(3) 
C28 0.021(3) 0.047(4) 0.010(3) -0.006(3) -0.002(2) -0.012(3) 
C29 0.016(3) 0.030(3) 0.029(4) -0.007(3) 0.012(3) 0.009(3) 
C30 0.010(3) 0.015(3) 0.027(3) -0.014(2) 0.002(2) 0.002(2) 
C31 0.029(4) 0.041(4) 0.028(3) -0.020(3) 0.003(3) -0.005(3) 
C32 0.005(3) 0.037(4) 0.037(4) -0.005(3) 0.000(3) -0.005(3) 
C33 0.001(3) 0.024(3) 0.026(4) -0.002(3) 0.002(2) -0.003(2) 
C34 0.013(3) 0.024(3) 0.030(3) 0.006(2) 0.005(3) -0.008(2) 
C35 0.014(4) 0.032(4) 0.033(4) 0.001(3) -0.001(3) 0.009(3) 
C36 0.029(4) 0.020(3) 0.013(3) -0.004(2) -0.011(3) 0.000(2) 
C37 0.020(4) 0.037(4) 0.013(3) 0.005(2) -0.005(2) 0.004(3) 
C38 0.022(4) 0.050(4) 0.019(4) -0.003(3) -0.003(3) 0.003(3) 
C39 0.013(3) 0.040(4) 0.034(4) -0.008(3) 0.008(3) 0.014(3) 
C40 0.011(3) 0.028(4) 0.028(3) -0.011(3) -0.008(2) -0.003(3) 
C101 0.033(5) 0.068(6) 0.038(5) 0.009(4) 0.001(4) 0.006(4) 
C102 0.040(5) 0.054(5) 0.044(5) 0.004(4) -0.001(4) 0.013(4) 
C103 0.067(6) 0.053(5) 0.062(6) -0.021(4) 0.004(5) 0.045(4) 
C104 0.035(4) 0.032(4) 0.026(3) 0.000(3) -0.019(3) 0.002(3) 
C105 0.056(6) 0.049(5) 0.062(6) -0.006(4) -0.036(5) -0.013(4) 
C106 0.039(5) 0.044(4) 0.083(7) 0.004(4) -0.003(4) -0.015(3) 
C107 0.032(4) 0.062(5) 0.058(5) 0.024(4) -0.011(3) -0.014(3) 
C108 0.021(4) 0.053(6) 0.042(5) -0.006(4) -0.006(4) 0.005(3) 
C109 0.042(5) 0.102(7) 0.038(5) -0.025(5) 0.003(4) 0.040(5) 
C110 0.051(5) 0.038(4) 0.028(4) -0.011(3) -0.021(3) 0.007(3) 
C111 0.041(5) 0.051(5) 0.037(4) -0.011(3) -0.024(4) 0.008(4) 
C112 0.061(6) 0.035(4) 0.058(6) 0.004(4) -0.017(5) 0.014(4) 
C113 0.045(6) 0.129(9) 0.066(7) 0.046(6) -0.021(5) -0.023(6) 
C114 0.047(6) 0.102(8) 0.092(8) -0.002(6) 0.031(5) 0.024(5) 
C115 0.028(4) 0.030(4) 0.029(4) 0.001(3) -0.002(3) 0.006(3) 
C116 0.025(4) 0.048(4) 0.024(4) -0.014(3) -0.019(3) 0.007(3) 
C201 0.025(4) 0.081(6) 0.031(4) -0.002(4) 0.004(3) -0.012(4) 
C202 0.050(5) 0.068(6) 0.041(5) 0.022(4) 0.003(4) 0.026(4) 
C203 0.042(5) 0.040(4) 0.056(5) 0.004(4) -0.002(4) -0.015(4) 
C204 0.028(4) 0.032(4) 0.049(4) -0.003(3) 0.003(3) 0.001(3) 
C205 0.046(5) 0.029(4) 0.071(6) -0.021(4) 0.010(4) -0.002(3) 
C206 0.029(3) 0.029(3) 0.055(5) -0.013(3) 0.001(3) -0.001(2) 
C207 0.026(4) 0.027(4) 0.053(5) -0.005(3) 0.010(4) 0.005(3) 
C208 0.059(6) 0.038(4) 0.041(5) 0.001(3) 0.012(4) 0.002(3) 
C209 0.053(5) 0.053(5) 0.048(5) 0.013(4) 0.008(4) -0.026(4) 
C210 0.048(5) 0.026(4) 0.073(6) 0.019(4) 0.021(4) 0.010(3) 
C211 0.034(4) 0.023(3) 0.044(4) 0.007(3) 0.011(3) -0.004(3) 
C212 0.043(4) 0.023(3) 0.055(5) 0.002(3) 0.009(3) 0.006(3) 
C213 0.056(5) 0.045(4) 0.037(4) -0.014(3) 0.017(3) -0.008(3) 
C214 0.033(5) 0.049(5) 0.024(4) -0.007(3) 0.007(3) -0.008(3) 
C215 0.019(4) 0.040(4) 0.022(4) -0.007(3) 0.002(3) -0.010(3) 
C216 0.038(5) 0.015(3) 0.055(5) 0.006(3) 0.013(4) 0.004(3) 
C301 0.029(4) 0.089(6) 0.067(6) -0.026(5) -0.014(4) 0.010(4) 
C302 0.058(5) 0.044(4) 0.061(5) -0.026(4) -0.017(4) 0.032(4) 
C303 0.056(5) 0.007(2) 0.039(4) -0.001(2) -0.019(3) 0.006(2) 
C304 0.041(4) 0.030(4) 0.027(3) 0.004(3) 0.003(3) -0.006(3) 
C305 0.041(5) 0.029(4) 0.064(5) 0.018(4) -0.004(4) -0.013(3) 
C306 0.061(5) 0.051(5) 0.043(5) 0.005(4) -0.005(4) 0.012(4) 
C307 0.049(5) 0.041(4) 0.042(5) 0.010(4) -0.013(4) -0.006(4) 
C308 0.060(5) 0.035(4) 0.044(4) 0.009(3) 0.013(3) 0.009(3) 
C309 0.065(5) 0.048(4) 0.042(4) 0.012(3) -0.008(4) -0.015(3) 
C310 0.075(6) 0.086(7) 0.041(5) 0.016(4) -0.024(5) -0.024(5) 
C311 0.059(5) 0.026(4) 0.041(4) -0.003(3) -0.041(4) 0.009(4) 
C312 0.046(5) 0.049(5) 0.031(4) 0.013(3) -0.008(4) -0.021(4) 
C313 0.031(4) 0.069(6) 0.053(5) 0.007(4) 0.012(3) -0.031(4) 
C314 0.021(4) 0.057(5) 0.038(4) -0.013(4) 0.002(3) -0.001(3) 
C315 0.031(4) 0.026(3) 0.021(3) -0.008(3) -0.006(3) -0.006(3) 
C316 0.026(4) 0.051(5) 0.030(4) 0.019(3) -0.017(3) -0.001(3) 
C401 0.028(4) 0.053(5) 0.041(5) 0.008(3) 0.003(3) 0.008(3) 
C402 0.039(4) 0.066(5) 0.026(3) -0.003(3) 0.000(3) -0.005(4) 
C403 0.031(4) 0.032(4) 0.070(6) 0.004(4) 0.020(4) 0.008(3) 
C404 0.026(4) 0.041(4) 0.040(4) 0.001(3) 0.009(3) -0.006(3) 
C405 0.042(5) 0.023(4) 0.073(6) 0.028(4) 0.018(4) 0.008(3) 
C406 0.026(4) 0.021(3) 0.052(5) 0.002(3) 0.010(3) 0.004(2) 
C407 0.021(4) 0.027(3) 0.047(5) 0.006(3) 0.010(3) -0.003(3) 
C408 0.038(5) 0.045(5) 0.040(5) -0.003(3) 0.012(3) 0.000(3) 
C409 0.037(4) 0.030(3) 0.066(5) -0.026(3) 0.009(4) 0.009(3) 
C410 0.039(4) 0.036(4) 0.042(4) -0.021(3) -0.007(3) 0.000(3) 
C411 0.024(3) 0.019(3) 0.046(4) -0.003(3) 0.010(3) 0.007(2) 
C412 0.033(4) 0.031(4) 0.046(5) -0.012(3) 0.003(3) -0.003(3) 
C413 0.048(5) 0.045(5) 0.037(4) 0.017(3) 0.012(3) 0.009(3) 
C414 0.032(4) 0.039(4) 0.030(4) -0.008(3) 0.005(3) 0.011(3) 
C415 0.028(4) 0.024(4) 0.039(5) -0.001(3) 0.004(3) -0.001(3) 
C416 0.020(4) 0.032(4) 0.038(4) 0.002(3) 0.008(3) 0.009(3) 
 
_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 2.087(5) . ? 
Ni1 O1 2.111(6) . ? 
Ni1 N5 2.124(6) . ? 
Ni1 N4 2.136(5) . ? 
Ni1 N1 2.139(5) 1_565 ? 
Ni1 N6 2.135(5) 1_455 ? 
Ni2 O7 2.066(5) . ? 
Ni2 N7 2.092(6) . ? 
Ni2 O10 2.110(5) . ? 
Ni2 N3 2.125(6) . ? 
Ni2 N8 2.148(6) 1_655 ? 
Ni2 N2 2.150(5) . ? 
O1 N9 1.277(8) . ? 
O2 N9 1.229(7) . ? 
O3 N9 1.140(7) . ? 
O4 N10 1.308(7) . ? 
O5 N10 1.230(7) . ? 
O6 N10 1.204(6) . ? 
O7 N11 1.256(8) . ? 
O8 N11 1.357(8) . ? 
O9 N11 1.112(8) . ? 
O10 N12 1.159(8) . ? 
O11 N12 1.142(8) . ? 
O12 N12 1.392(9) . ? 
N1 C1 1.270(8) . ? 
N1 C5 1.399(8) . ? 
N1 Ni1 2.139(5) 1_545 ? 
N2 C8 1.287(8) . ? 
N2 C10 1.391(8) . ? 
N3 C11 1.277(9) . ? 
N3 C15 1.413(8) . ? 
N4 C20 1.300(8) . ? 
N4 C18 1.398(7) . ? 
N5 C25 1.280(8) . ? 
N5 C21 1.376(9) . ? 
N6 C30 1.340(8) . ? 
N6 C28 1.395(8) . ? 
N6 Ni1 2.135(5) 1_655 ? 
N7 C40 1.307(9) . ? 
N7 C31 1.393(8) . ? 
N8 C34 1.284(9) . ? 
N8 C38 1.355(9) . ? 
N8 Ni2 2.148(6) 1_455 ? 
C1 C2 1.391(10) . ? 
C2 C3 1.346(9) . ? 
C3 C4 1.450(8) . ? 
C3 C6 1.473(9) . ? 
C4 C5 1.370(9) . ? 
C6 C9 1.354(9) . ? 
C6 C7 1.429(8) . ? 
C7 C8 1.383(9) . ? 
C9 C10 1.388(9) . ? 
C11 C12 1.392(10) . ? 
C12 C13 1.321(9) . ? 
C13 C14 1.444(9) . ? 
C13 C16 1.498(9) . ? 
C14 C15 1.361(9) . ? 
C16 C17 1.338(9) . ? 
C16 C19 1.422(8) . ? 
C17 C18 1.388(9) . ? 
C19 C20 1.366(9) . ? 
C21 C22 1.364(9) . ? 
C22 C23 1.417(9) . ? 
C23 C24 1.423(10) . ? 
C23 C26 1.517(9) . ? 
C24 C25 1.412(9) . ? 
C26 C29 1.317(10) . ? 
C26 C27 1.394(9) . ? 
C27 C28 1.339(9) . ? 
C29 C30 1.402(9) . ? 
C31 C32 1.344(9) . ? 
C32 C33 1.358(10) . ? 
C33 C39 1.351(10) . ? 
C33 C36 1.453(9) . ? 
C34 C35 1.430(9) . ? 
C35 C36 1.383(10) . ? 
C36 C37 1.463(9) . ? 
C37 C38 1.378(9) . ? 
C39 C40 1.398(8) . ? 
C101 C114 1.367(14) . ? 
C101 C102 1.460(12) . ? 
C101 C116 1.401(12) . ? 
C102 C103 1.295(13) . ? 
C103 C104 1.443(12) . ? 
C104 C105 1.446(12) . ? 
C104 C115 1.435(10) . ? 
C105 C106 1.438(13) . ? 
C106 C107 1.332(12) . ? 
C107 C108 1.380(11) . ? 
C108 C115 1.437(12) . ? 
C108 C109 1.419(13) . ? 
C109 C110 1.375(14) . ? 
C110 C111 1.444(12) . ? 
C111 C112 1.364(14) . ? 
C111 C116 1.399(12) . ? 
C112 C113 1.312(14) . ? 
C113 C114 1.41(2) . ? 
C115 C116 1.422(4) . ? 
C201 C202 1.325(12) . ? 
C201 C214 1.431(12) . ? 
C202 C203 1.385(12) . ? 
C203 C204 1.384(12) . ? 
C204 C215 1.387(11) . ? 
C204 C205 1.454(11) . ? 
C205 C206 1.302(12) . ? 
C206 C207 1.514(10) . ? 
C207 C208 1.357(12) . ? 
C207 C216 1.406(11) . ? 
C208 C209 1.434(11) . ? 
C209 C210 1.370(13) . ? 
C210 C211 1.422(12) . ? 
C211 C212 1.433(11) . ? 
C211 C216 1.438(10) . ? 
C212 C213 1.383(11) . ? 
C213 C214 1.346(11) . ? 
C214 C215 1.459(10) . ? 
C215 C216 1.425(4) . ? 
C301 C302 1.389(13) . ? 
C301 C314 1.402(12) . ? 
C302 C303 1.413(11) . ? 
C303 C304 1.435(9) . ? 
C304 C315 1.427(9) . ? 
C304 C305 1.471(11) . ? 
C305 C306 1.330(13) . ? 
C306 C307 1.411(13) . ? 
C307 C308 1.398(13) . ? 
C307 C316 1.417(12) . ? 
C308 C309 1.371(11) . ? 
C309 C310 1.346(12) . ? 
C310 C311 1.316(12) . ? 
C311 C312 1.405(12) . ? 
C311 C316 1.429(11) . ? 
C312 C313 1.328(13) . ? 
C313 C314 1.423(11) . ? 
C314 C315 1.426(10) . ? 
C315 C316 1.414(4) . ? 
C401 C402 1.314(11) . ? 
C401 C414 1.425(12) . ? 
C402 C403 1.446(12) . ? 
C403 C404 1.342(12) . ? 
C404 C416 1.382(11) . ? 
C404 C405 1.500(11) . ? 
C405 C406 1.307(11) . ? 
C406 C407 1.509(10) . ? 
C407 C408 1.362(12) . ? 
C407 C415 1.448(11) . ? 
C408 C409 1.437(11) . ? 
C409 C410 1.351(12) . ? 
C410 C411 1.429(10) . ? 
C411 C412 1.386(11) . ? 
C411 C415 1.465(10) . ? 
C412 C413 1.388(10) . ? 
C413 C414 1.352(11) . ? 
C414 C416 1.424(11) . ? 
C415 C416 1.425(4) . ? 
 
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 O1 169.8(2) . . ? 
O4 Ni1 N5 93.4(2) . . ? 
O1 Ni1 N5 96.7(2) . . ? 
O4 Ni1 N4 85.3(2) . . ? 
O1 Ni1 N4 93.6(2) . . ? 
N5 Ni1 N4 91.2(2) . . ? 
O4 Ni1 N1 92.9(2) . 1_565 ? 
O1 Ni1 N1 88.5(2) . 1_565 ? 
N5 Ni1 N1 86.9(2) . 1_565 ? 
N4 Ni1 N1 177.3(2) . 1_565 ? 
O4 Ni1 N6 85.5(2) . 1_455 ? 
O1 Ni1 N6 84.4(2) . 1_455 ? 
N5 Ni1 N6 176.6(2) . 1_455 ? 
N4 Ni1 N6 91.9(2) . 1_455 ? 
N1 Ni1 N6 90.0(2) 1_565 1_455 ? 
O7 Ni2 N7 95.9(2) . . ? 
O7 Ni2 O10 171.5(2) . . ? 
N7 Ni2 O10 92.5(2) . . ? 
O7 Ni2 N3 86.5(2) . . ? 
N7 Ni2 N3 89.6(2) . . ? 
O10 Ni2 N3 94.5(2) . . ? 
O7 Ni2 N8 83.4(2) . 1_655 ? 
N7 Ni2 N8 176.7(2) . 1_655 ? 
O10 Ni2 N8 88.2(2) . 1_655 ? 
N3 Ni2 N8 87.2(2) . 1_655 ? 
O7 Ni2 N2 92.4(2) . . ? 
N7 Ni2 N2 91.6(2) . . ? 
O10 Ni2 N2 86.4(2) . . ? 
N3 Ni2 N2 178.5(2) . . ? 
N8 Ni2 N2 91.6(2) 1_655 . ? 
N9 O1 Ni1 136.8(5) . . ? 
N10 O4 Ni1 142.2(4) . . ? 
N11 O7 Ni2 143.5(5) . . ? 
N12 O10 Ni2 149.1(5) . . ? 
C1 N1 C5 118.2(5) . . ? 
C1 N1 Ni1 124.3(4) . 1_545 ? 
C5 N1 Ni1 117.5(4) . 1_545 ? 
C8 N2 C10 116.2(6) . . ? 
C8 N2 Ni2 122.5(4) . . ? 
C10 N2 Ni2 121.2(4) . . ? 
C11 N3 C15 114.5(6) . . ? 
C11 N3 Ni2 123.5(5) . . ? 
C15 N3 Ni2 121.8(4) . . ? 
C20 N4 C18 115.9(5) . . ? 
C20 N4 Ni1 124.0(4) . . ? 
C18 N4 Ni1 120.1(4) . . ? 
C25 N5 C21 118.5(6) . . ? 
C25 N5 Ni1 121.3(4) . . ? 
C21 N5 Ni1 120.2(5) . . ? 
C30 N6 C28 115.8(5) . . ? 
C30 N6 Ni1 121.2(4) . 1_655 ? 
C28 N6 Ni1 122.9(4) . 1_655 ? 
C40 N7 C31 114.5(6) . . ? 
C40 N7 Ni2 122.0(5) . . ? 
C31 N7 Ni2 123.5(5) . . ? 
C34 N8 C38 116.2(6) . . ? 
C34 N8 Ni2 123.4(5) . 1_455 ? 
C38 N8 Ni2 120.4(5) . 1_455 ? 
O3 N9 O2 121.1(7) . . ? 
O3 N9 O1 123.4(6) . . ? 
O2 N9 O1 115.3(5) . . ? 
O6 N10 O5 122.9(6) . . ? 
O6 N10 O4 120.1(6) . . ? 
O5 N10 O4 116.4(5) . . ? 
O9 N11 O7 128.4(8) . . ? 
O9 N11 O8 118.8(7) . . ? 
O7 N11 O8 112.6(6) . . ? 
O11 N12 O10 136.5(8) . . ? 
O11 N12 O12 110.3(7) . . ? 
O10 N12 O12 111.4(7) . . ? 
N1 C1 C2 123.1(6) . . ? 
C1 C2 C3 122.1(6) . . ? 
C2 C3 C4 116.0(5) . . ? 
C2 C3 C6 126.2(6) . . ? 
C4 C3 C6 117.7(6) . . ? 
C5 C4 C3 118.4(6) . . ? 
N1 C5 C4 121.9(6) . . ? 
C9 C6 C7 115.6(6) . . ? 
C9 C6 C3 123.4(5) . . ? 
C7 C6 C3 120.8(6) . . ? 
C8 C7 C6 117.8(6) . . ? 
N2 C8 C7 126.8(6) . . ? 
C6 C9 C10 123.1(6) . . ? 
C9 C10 N2 120.4(6) . . ? 
N3 C11 C12 125.0(7) . . ? 
C13 C12 C11 121.8(6) . . ? 
C12 C13 C14 116.9(6) . . ? 
C12 C13 C16 126.0(6) . . ? 
C14 C13 C16 117.0(6) . . ? 
C15 C14 C13 117.2(6) . . ? 
C14 C15 N3 124.3(6) . . ? 
C17 C16 C19 117.2(6) . . ? 
C17 C16 C13 123.8(5) . . ? 
C19 C16 C13 118.7(6) . . ? 
C16 C17 C18 122.5(6) . . ? 
C17 C18 N4 120.1(6) . . ? 
C20 C19 C16 117.3(6) . . ? 
N4 C20 C19 126.9(6) . . ? 
C22 C21 N5 123.9(7) . . ? 
C21 C22 C23 118.0(6) . . ? 
C24 C23 C22 117.7(7) . . ? 
C24 C23 C26 119.8(6) . . ? 
C22 C23 C26 122.4(6) . . ? 
C23 C24 C25 118.2(6) . . ? 
N5 C25 C24 123.6(6) . . ? 
C29 C26 C27 118.3(6) . . ? 
C29 C26 C23 122.2(6) . . ? 
C27 C26 C23 119.5(6) . . ? 
C28 C27 C26 120.1(6) . . ? 
C27 C28 N6 122.7(6) . . ? 
C26 C29 C30 121.1(7) . . ? 
N6 C30 C29 121.9(6) . . ? 
C32 C31 N7 122.9(6) . . ? 
C31 C32 C33 122.0(7) . . ? 
C39 C33 C32 115.6(6) . . ? 
C39 C33 C36 123.0(6) . . ? 
C32 C33 C36 121.3(6) . . ? 
N8 C34 C35 125.1(6) . . ? 
C36 C35 C34 119.4(6) . . ? 
C35 C36 C37 116.1(6) . . ? 
C35 C36 C33 121.2(6) . . ? 
C37 C36 C33 122.6(6) . . ? 
C38 C37 C36 117.3(7) . . ? 
N8 C38 C37 125.9(7) . . ? 
C33 C39 C40 121.3(6) . . ? 
N7 C40 C39 123.5(6) . . ? 
C114 C101 C102 119.5(9) . . ? 
C114 C101 C116 119.2(9) . . ? 
C102 C101 C116 121.3(9) . . ? 
C103 C102 C101 118.4(8) . . ? 
C102 C103 C104 124.3(8) . . ? 
C105 C104 C115 118.5(8) . . ? 
C105 C104 C103 123.7(8) . . ? 
C115 C104 C103 117.3(8) . . ? 
C104 C105 C106 117.8(8) . . ? 
C107 C106 C105 121.9(8) . . ? 
C106 C107 C108 122.4(9) . . ? 
C107 C108 C115 119.5(8) . . ? 
C107 C108 C109 124.5(9) . . ? 
C115 C108 C109 115.9(8) . . ? 
C110 C109 C108 123.7(8) . . ? 
C109 C110 C111 120.3(8) . . ? 
C112 C111 C116 119.1(10) . . ? 
C112 C111 C110 123.1(9) . . ? 
C116 C111 C110 117.6(9) . . ? 
C113 C112 C111 121.5(10) . . ? 
C112 C113 C114 121.0(10) . . ? 
C101 C114 C113 119.1(10) . . ? 
C108 C115 C116 120.8(5) . . ? 
C108 C115 C104 119.5(8) . . ? 
C116 C115 C104 119.7(5) . . ? 
C111 C116 C115 121.6(6) . . ? 
C111 C116 C101 119.7(9) . . ? 
C115 C116 C101 118.7(6) . . ? 
C202 C201 C214 123.3(9) . . ? 
C201 C202 C203 122.2(9) . . ? 
C202 C203 C204 118.6(8) . . ? 
C215 C204 C203 120.6(8) . . ? 
C215 C204 C205 116.1(8) . . ? 
C203 C204 C205 122.9(8) . . ? 
C206 C205 C204 124.9(8) . . ? 
C205 C206 C207 120.1(8) . . ? 
C208 C207 C216 123.9(7) . . ? 
C208 C207 C206 120.7(8) . . ? 
C216 C207 C206 115.2(7) . . ? 
C207 C208 C209 118.9(8) . . ? 
C210 C209 C208 118.6(8) . . ? 
C209 C210 C211 123.3(8) . . ? 
C212 C211 C210 122.7(7) . . ? 
C212 C211 C216 120.0(7) . . ? 
C210 C211 C216 117.3(8) . . ? 
C211 C212 C213 118.0(7) . . ? 
C214 C213 C212 123.9(7) . . ? 
C213 C214 C201 125.7(7) . . ? 
C213 C214 C215 120.6(7) . . ? 
C201 C214 C215 113.6(7) . . ? 
C204 C215 C216 121.4(5) . . ? 
C204 C215 C214 121.2(8) . . ? 
C216 C215 C214 117.4(5) . . ? 
C207 C216 C215 122.3(5) . . ? 
C207 C216 C211 117.8(8) . . ? 
C215 C216 C211 119.8(6) . . ? 
C302 C301 C314 121.1(8) . . ? 
C303 C302 C301 122.3(7) . . ? 
C302 C303 C304 117.8(6) . . ? 
C303 C304 C315 119.6(6) . . ? 
C303 C304 C305 123.3(6) . . ? 
C315 C304 C305 117.0(7) . . ? 
C306 C305 C304 120.3(8) . . ? 
C305 C306 C307 124.6(9) . . ? 
C308 C307 C306 124.9(9) . . ? 
C308 C307 C316 118.8(8) . . ? 
C306 C307 C316 116.2(9) . . ? 
C309 C308 C307 119.2(8) . . ? 
C310 C309 C308 120.7(9) . . ? 
C311 C310 C309 124.0(9) . . ? 
C310 C311 C312 122.0(8) . . ? 
C310 C311 C316 118.2(9) . . ? 
C312 C311 C316 119.7(7) . . ? 
C313 C312 C311 121.6(7) . . ? 
C312 C313 C314 121.4(7) . . ? 
C301 C314 C315 118.3(8) . . ? 
C301 C314 C313 122.6(8) . . ? 
C315 C314 C313 119.0(7) . . ? 
C314 C315 C316 119.4(5) . . ? 
C314 C315 C304 120.9(7) . . ? 
C316 C315 C304 119.7(5) . . ? 
C311 C316 C315 118.9(5) . . ? 
C311 C316 C307 119.0(8) . . ? 
C315 C316 C307 122.1(6) . . ? 
C402 C401 C414 123.1(9) . . ? 
C401 C402 C403 122.1(8) . . ? 
C404 C403 C402 116.3(8) . . ? 
C403 C404 C416 122.3(8) . . ? 
C403 C404 C405 121.3(8) . . ? 
C416 C404 C405 116.2(8) . . ? 
C406 C405 C404 123.7(8) . . ? 
C405 C406 C407 121.8(8) . . ? 
C408 C407 C415 123.1(7) . . ? 
C408 C407 C406 123.0(7) . . ? 
C415 C407 C406 113.6(7) . . ? 
C407 C408 C409 119.6(8) . . ? 
C410 C409 C408 118.7(7) . . ? 
C409 C410 C411 124.6(7) . . ? 
C412 C411 C410 123.8(7) . . ? 
C412 C411 C415 119.3(7) . . ? 
C410 C411 C415 116.9(7) . . ? 
C411 C412 C413 119.6(7) . . ? 
C414 C413 C412 121.9(7) . . ? 
C413 C414 C401 123.7(8) . . ? 
C413 C414 C416 122.5(7) . . ? 
C401 C414 C416 113.7(7) . . ? 
C416 C415 C407 123.3(5) . . ? 
C416 C415 C411 119.9(5) . . ? 
C407 C415 C411 116.7(7) . . ? 
C404 C416 C415 121.2(6) . . ? 
C404 C416 C414 122.3(8) . . ? 
C415 C416 C414 116.5(5) . . ? 
 
_refine_diff_density_max    0.751 
_refine_diff_density_min   -0.658 
_refine_diff_density_rms    0.058 
#==============================================================================