# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008


data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Franc Meyer'
'Sebastian Dechert'
'Serhiy Demeshko'
'Sebastian Fuchs'
'Feng-Mei Nie.'
'Thomas Pruschke'

_publ_contact_author_name        'Franc Meyer'
_publ_contact_author_email       FRANC.MEYER@CHEMIE.UNI-GOETTINGEN.DE

_publ_section_title              
;
Targeted self-assembly and quantum Monte Carlo
magnetic study of an alternating nickel(II) 1D coordination polymer
composed of highly preorganized binuclear tectons
;

# Attachment 'Meyer_et_al.CIF'

#==============================================================================
data_1-k138-1
_database_code_depnum_ccdc_archive 'CCDC 682091'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H45 N11 Ni2 O2 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C35 H45 Cl2 N11 Ni2 O10'
_chemical_formula_weight         968.14

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3837(5)
_cell_length_b                   12.5115(8)
_cell_length_c                   19.9157(13)
_cell_angle_alpha                81.243(5)
_cell_angle_beta                 81.304(5)
_cell_angle_gamma                79.630(5)
_cell_volume                     2014.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    30089
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      24.68

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1004
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(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  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30089
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         24.68
_reflns_number_total             6812
_reflns_number_gt                5196
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (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^)+(0.0996P)^2^+1.8211P] 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         6812
_refine_ls_number_parameters     537
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.001
_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
Ni1 Ni 0.57743(8) 0.32308(5) 0.79940(4) 0.0389(2) Uani 1 1 d . . .
Ni2 Ni 0.52235(7) 0.65371(5) 0.66968(3) 0.0332(2) Uani 1 1 d . A .
Cl1 Cl 0.93664(18) 0.79193(12) 0.44165(8) 0.0573(4) Uani 1 1 d D . .
Cl2 Cl 0.69367(16) 0.74739(12) 0.93333(7) 0.0474(3) Uani 1 1 d . . .
N1 N 0.5006(5) 0.3936(3) 0.7081(2) 0.0376(10) Uani 1 1 d . A .
N2 N 0.4871(5) 0.4939(3) 0.6685(2) 0.0374(10) Uani 1 1 d . . .
N3 N 0.4298(6) 0.2080(3) 0.7882(3) 0.0491(12) Uani 1 1 d D A .
N4 N 0.3926(5) 0.4183(3) 0.8573(2) 0.0389(10) Uani 1 1 d . A .
N6 N 0.3395(6) 0.6819(4) 0.5997(2) 0.0419(10) Uani 1 1 d . . .
N7 N 0.3493(5) 0.7088(3) 0.7491(2) 0.0330(9) Uani 1 1 d . . .
N8 N 0.5844(5) 0.8149(3) 0.6427(2) 0.0399(10) Uani 1 1 d . . .
N9 N 0.7476(6) 0.4290(4) 0.7907(3) 0.0504(12) Uani 1 1 d . A .
N10 N 0.7205(5) 0.5207(4) 0.7639(2) 0.0421(11) Uani 1 1 d . . .
N11 N 0.6986(5) 0.6099(4) 0.7367(3) 0.0448(11) Uani 1 1 d . A .
O1 O 0.7777(5) 0.2190(3) 0.7351(2) 0.0609(12) Uani 1 1 d D A .
O2 O 0.7177(6) 0.6180(3) 0.5873(2) 0.0625(13) Uani 1 1 d D . .
C1 C 0.3796(8) 0.3807(5) 0.6172(3) 0.0551(15) Uani 1 1 d . . .
H1A H 0.3291 0.3532 0.5866 0.080 Uiso 1 1 calc R A .
C2 C 0.4359(7) 0.3268(5) 0.6773(3) 0.0500(15) Uani 1 1 d . A .
C3 C 0.4160(7) 0.4847(5) 0.6135(3) 0.0454(13) Uani 1 1 d . A .
C4 C 0.4308(9) 0.2126(5) 0.7128(3) 0.0609(17) Uani 1 1 d . . .
H4A H 0.3336 0.1879 0.7041 0.080 Uiso 1 1 calc R A .
H4B H 0.5254 0.1637 0.6946 0.080 Uiso 1 1 calc R . .
C5 C 0.2615(7) 0.2328(5) 0.8230(4) 0.0631(19) Uani 1 1 d . . .
H5A H 0.2634 0.2133 0.8720 0.080 Uiso 1 1 calc R A .
H5B H 0.1948 0.1868 0.8086 0.080 Uiso 1 1 calc R . .
C6 C 0.1806(7) 0.3516(5) 0.8097(4) 0.0551(16) Uani 1 1 d . A .
H6A H 0.2082 0.3786 0.7618 0.080 Uiso 1 1 calc R . .
H6B H 0.0629 0.3551 0.8184 0.080 Uiso 1 1 calc R . .
C7 C 0.2310(6) 0.4246(4) 0.8531(3) 0.0430(13) Uani 1 1 d . . .
C8 C 0.1151(8) 0.4935(5) 0.8900(3) 0.0550(16) Uani 1 1 d . A .
H8 H 0.0050 0.4953 0.8872 0.080 Uiso 1 1 calc R . .
C9 C 0.1589(8) 0.5594(5) 0.9307(3) 0.0567(16) Uani 1 1 d . . .
H9 H 0.0802 0.6066 0.9548 0.080 Uiso 1 1 calc R A .
C10 C 0.3237(8) 0.5537(5) 0.9349(3) 0.0541(15) Uani 1 1 d . A .
H10 H 0.3584 0.5968 0.9622 0.080 Uiso 1 1 calc R . .
C11 C 0.4356(8) 0.4825(5) 0.8976(3) 0.0480(14) Uani 1 1 d . . .
H11 H 0.5461 0.4789 0.9005 0.080 Uiso 1 1 calc R A .
C12A C 0.5016(15) 0.0964(7) 0.8222(8) 0.047(4) Uiso 0.58(3) 1 d PD A 1
H12A H 0.4316 0.0451 0.8171 0.080 Uiso 0.58(3) 1 calc PR A 1
H12B H 0.6068 0.0744 0.7961 0.080 Uiso 0.58(3) 1 calc PR A 1
C13A C 0.5273(16) 0.0810(10) 0.8968(8) 0.054(4) Uiso 0.58(3) 1 d PD A 1
H13A H 0.4266 0.1121 0.9227 0.080 Uiso 0.58(3) 1 calc PR A 1
H13B H 0.5461 0.0030 0.9123 0.080 Uiso 0.58(3) 1 calc PR A 1
C14A C 0.6646(18) 0.1298(8) 0.9144(6) 0.044(3) Uiso 0.58(3) 1 d PD A 1
C15A C 0.7621(19) 0.0700(9) 0.9629(6) 0.051(3) Uiso 0.58(3) 1 d PD A 1
H15A H 0.7510 -0.0020 0.9800 0.080 Uiso 0.58(3) 1 calc PR A 1
C16A C 0.874(2) 0.1201(10) 0.9845(6) 0.057(4) Uiso 0.58(3) 1 d PD A 1
H16A H 0.9404 0.0812 1.0165 0.080 Uiso 0.58(3) 1 calc PR A 1
C17A C 0.8903(17) 0.2274(12) 0.9597(6) 0.054(3) Uiso 0.58(3) 1 d PD A 1
H17A H 0.9636 0.2629 0.9750 0.080 Uiso 0.58(3) 1 calc PR A 1
C18A C 0.7931(15) 0.2783(11) 0.9115(5) 0.040(3) Uiso 0.58(3) 1 d PD A 1
H18A H 0.8057 0.3497 0.8931 0.080 Uiso 0.58(3) 1 calc PR A 1
N5A N 0.6832(14) 0.2354(9) 0.8887(6) 0.046(4) Uiso 0.58(3) 1 d PD A 1
C12B C 0.4916(19) 0.0896(8) 0.8031(10) 0.043(5) Uiso 0.42(3) 1 d PD A 2
H12C H 0.5984 0.0704 0.7776 0.080 Uiso 0.42(3) 1 calc PR A 2
H12D H 0.4172 0.0461 0.7916 0.080 Uiso 0.42(3) 1 calc PR A 2
C13B C 0.5011(19) 0.0721(12) 0.8784(9) 0.047(5) Uiso 0.42(3) 1 d PD A 2
H13C H 0.3950 0.1018 0.9009 0.080 Uiso 0.42(3) 1 calc PR A 2
H13D H 0.5177 -0.0063 0.8927 0.080 Uiso 0.42(3) 1 calc PR A 2
C14B C 0.627(2) 0.1180(10) 0.9060(7) 0.040(5) Uiso 0.42(3) 1 d PD A 2
C15B C 0.709(2) 0.0527(11) 0.9578(7) 0.046(4) Uiso 0.42(3) 1 d PD A 2
H15B H 0.6887 -0.0184 0.9722 0.080 Uiso 0.42(3) 1 calc PR A 2
C16B C 0.818(2) 0.0934(11) 0.9872(6) 0.040(4) Uiso 0.42(3) 1 d PD A 2
H16B H 0.8677 0.0518 1.0236 0.080 Uiso 0.42(3) 1 calc PR A 2
C17B C 0.855(2) 0.1973(13) 0.9625(7) 0.044(4) Uiso 0.42(3) 1 d PD A 2
H17B H 0.9322 0.2267 0.9801 0.080 Uiso 0.42(3) 1 calc PR A 2
C18B C 0.772(2) 0.2532(15) 0.9109(8) 0.051(6) Uiso 0.42(3) 1 d PD A 2
H18B H 0.7938 0.3236 0.8951 0.080 Uiso 0.42(3) 1 calc PR A 2
N5B N 0.6641(16) 0.2197(10) 0.8805(7) 0.031(4) Uiso 0.42(3) 1 d PD A 2
C19 C 0.3876(8) 0.5834(5) 0.5626(3) 0.0523(15) Uani 1 1 d . A .
H19A H 0.3015 0.5773 0.5366 0.080 Uiso 1 1 calc R . .
H19B H 0.4864 0.5902 0.5310 0.080 Uiso 1 1 calc R . .
C20 C 0.1644(7) 0.6849(5) 0.6318(3) 0.0469(13) Uani 1 1 d . A .
H20A H 0.1104 0.6459 0.6057 0.080 Uiso 1 1 calc R . .
H20B H 0.1105 0.7606 0.6278 0.080 Uiso 1 1 calc R . .
C21 C 0.1401(6) 0.6363(5) 0.7063(3) 0.0425(12) Uani 1 1 d . . .
H21A H 0.0259 0.6293 0.7194 0.080 Uiso 1 1 calc R A .
H21B H 0.2039 0.5635 0.7116 0.080 Uiso 1 1 calc R . .
C22 C 0.1889(6) 0.7037(4) 0.7531(3) 0.0367(11) Uani 1 1 d . A .
C23 C 0.0727(7) 0.7613(5) 0.7974(3) 0.0468(13) Uani 1 1 d . . .
H23 H -0.0375 0.7578 0.7985 0.080 Uiso 1 1 calc R A .
C24 C 0.1206(8) 0.8238(5) 0.8400(3) 0.0534(15) Uani 1 1 d . A .
H24 H 0.0437 0.8644 0.8689 0.080 Uiso 1 1 calc R . .
C25 C 0.2863(8) 0.8244(5) 0.8385(3) 0.0477(14) Uani 1 1 d . . .
H25 H 0.3233 0.8625 0.8681 0.080 Uiso 1 1 calc R A .
C26 C 0.3950(7) 0.7674(4) 0.7923(3) 0.0389(12) Uani 1 1 d . A .
H26 H 0.5058 0.7694 0.7909 0.080 Uiso 1 1 calc R . .
C27 C 0.3520(8) 0.7829(5) 0.5505(3) 0.0508(14) Uani 1 1 d . A .
H27A H 0.2663 0.7941 0.5213 0.080 Uiso 1 1 calc R . .
H27B H 0.4564 0.7738 0.5217 0.080 Uiso 1 1 calc R . .
C28 C 0.3368(7) 0.8832(5) 0.5874(3) 0.0495(14) Uani 1 1 d . . .
H28A H 0.2954 0.9477 0.5575 0.080 Uiso 1 1 calc R A .
H28B H 0.2572 0.8763 0.6279 0.080 Uiso 1 1 calc R . .
C29 C 0.4946(7) 0.9002(4) 0.6085(3) 0.0417(13) Uani 1 1 d . A .
C30 C 0.5470(8) 1.0016(4) 0.5918(3) 0.0494(14) Uani 1 1 d . . .
H30 H 0.4822 1.0599 0.5689 0.080 Uiso 1 1 calc R A .
C31 C 0.6916(8) 1.0160(5) 0.6086(3) 0.0568(17) Uani 1 1 d . A .
H31 H 0.7277 1.0832 0.5965 0.080 Uiso 1 1 calc R . .
C32 C 0.7844(8) 0.9299(5) 0.6440(4) 0.0611(18) Uani 1 1 d . . .
H32 H 0.8833 0.9377 0.6569 0.080 Uiso 1 1 calc R A .
C33 C 0.7261(7) 0.8320(5) 0.6595(4) 0.0527(15) Uani 1 1 d . A .
H33 H 0.7890 0.7737 0.6832 0.080 Uiso 1 1 calc R . .
C34A C 0.9037(17) 0.1313(13) 0.7565(6) 0.069(4) Uiso 0.67(4) 1 d PD A 3
H34A H 0.9902 0.1218 0.7194 0.080 Uiso 0.67(4) 1 calc PR A 3
H34B H 0.8586 0.0648 0.7695 0.080 Uiso 0.67(4) 1 calc PR A 3
H34C H 0.9460 0.1491 0.7949 0.080 Uiso 0.67(4) 1 calc PR A 3
C34B C 0.9370(17) 0.182(3) 0.7510(10) 0.055(8) Uiso 0.33(4) 1 d PD A 4
H34D H 0.9330 0.1444 0.7968 0.080 Uiso 0.33(4) 1 calc PR A 4
H34E H 0.9929 0.2437 0.7477 0.080 Uiso 0.33(4) 1 calc PR A 4
H34F H 0.9942 0.1331 0.7195 0.080 Uiso 0.33(4) 1 calc PR A 4
C35 C 0.8306(8) 0.5164(5) 0.5874(4) 0.0605(18) Uani 1 1 d . A .
H35A H 0.9183 0.5194 0.6126 0.080 Uiso 1 1 calc R . .
H35B H 0.8740 0.5052 0.5411 0.080 Uiso 1 1 calc R . .
H35C H 0.7746 0.4569 0.6085 0.080 Uiso 1 1 calc R . .
O3A O 0.7648(8) 0.7916(7) 0.4660(4) 0.071(3) Uiso 0.550(9) 1 d PD B 5
O4A O 1.0342(13) 0.7322(9) 0.4890(5) 0.140(6) Uiso 0.550(9) 1 d PD B 5
O5A O 0.9654(10) 0.7289(6) 0.3807(4) 0.074(3) Uiso 0.550(9) 1 d PD B 5
O6A O 0.9641(11) 0.8983(6) 0.4171(5) 0.086(3) Uiso 0.550(9) 1 d PD B 5
O3B O 1.0996(10) 0.7537(8) 0.4091(5) 0.077(4) Uiso 0.450(9) 1 d PD B 6
O4B O 0.8269(12) 0.8364(9) 0.3971(5) 0.093(4) Uiso 0.450(9) 1 d PD B 6
O5B O 0.9626(15) 0.8762(9) 0.4814(6) 0.119(6) Uiso 0.450(9) 1 d PD B 6
O6B O 0.8895(17) 0.7034(10) 0.4899(7) 0.172(9) Uiso 0.450(9) 1 d PD B 6
O7 O 0.6981(6) 0.8234(4) 0.8709(2) 0.0660(12) Uani 1 1 d . . .
O8 O 0.5319(6) 0.7573(5) 0.9680(3) 0.0752(14) Uani 1 1 d . . .
O9 O 0.8014(7) 0.7720(5) 0.9757(3) 0.0830(16) Uani 1 1 d . . .
O10 O 0.7461(7) 0.6384(4) 0.9162(3) 0.0727(13) Uani 1 1 d . . .
H1 H 0.785(5) 0.248(4) 0.6956(16) 0.080 Uiso 1 1 d D . .
H2 H 0.751(9) 0.674(4) 0.569(4) 0.080 Uiso 1 1 d 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 0.0298(4) 0.0328(4) 0.0501(4) -0.0014(3) 0.0055(3) -0.0063(3)
Ni2 0.0272(3) 0.0322(3) 0.0391(4) -0.0053(3) 0.0029(3) -0.0068(3)
Cl1 0.0471(8) 0.0569(9) 0.0620(9) 0.0110(7) -0.0028(7) -0.0117(7)
Cl2 0.0335(7) 0.0546(8) 0.0545(8) -0.0157(6) -0.0002(6) -0.0056(6)
N1 0.034(2) 0.034(2) 0.045(2) -0.0100(18) 0.0036(19) -0.0090(18)
N2 0.033(2) 0.037(2) 0.041(2) -0.0080(18) 0.0055(19) -0.0087(18)
N3 0.040(3) 0.030(2) 0.074(3) -0.009(2) 0.008(2) -0.0076(19)
N4 0.033(2) 0.033(2) 0.048(3) -0.0019(19) 0.0019(19) -0.0060(18)
N6 0.044(3) 0.048(3) 0.034(2) -0.0068(19) -0.0026(19) -0.009(2)
N7 0.031(2) 0.033(2) 0.036(2) -0.0026(17) -0.0040(17) -0.0079(17)
N8 0.033(2) 0.033(2) 0.051(3) -0.0023(19) 0.0044(19) -0.0062(18)
N9 0.034(3) 0.046(3) 0.069(3) 0.008(2) -0.009(2) -0.012(2)
N10 0.023(2) 0.045(3) 0.059(3) -0.004(2) -0.003(2) -0.0099(19)
N11 0.033(2) 0.031(2) 0.073(3) -0.004(2) -0.014(2) -0.0065(19)
O1 0.058(3) 0.052(2) 0.063(3) -0.008(2) 0.014(2) -0.003(2)
O2 0.054(3) 0.047(2) 0.073(3) -0.007(2) 0.030(2) -0.005(2)
C1 0.066(4) 0.055(4) 0.051(4) -0.021(3) -0.004(3) -0.015(3)
C2 0.048(3) 0.038(3) 0.065(4) -0.021(3) 0.010(3) -0.012(3)
C3 0.046(3) 0.048(3) 0.043(3) -0.019(2) 0.003(3) -0.008(3)
C4 0.075(5) 0.042(3) 0.070(4) -0.019(3) 0.000(3) -0.020(3)
C5 0.039(3) 0.041(3) 0.106(5) -0.015(3) 0.019(3) -0.017(3)
C6 0.029(3) 0.045(3) 0.092(5) -0.018(3) 0.006(3) -0.012(2)
C7 0.034(3) 0.033(3) 0.055(3) 0.000(2) 0.010(2) -0.007(2)
C8 0.040(3) 0.039(3) 0.077(4) -0.003(3) 0.009(3) -0.002(3)
C9 0.055(4) 0.043(3) 0.063(4) -0.011(3) 0.013(3) 0.003(3)
C10 0.063(4) 0.049(3) 0.050(3) -0.011(3) -0.006(3) -0.004(3)
C11 0.047(3) 0.046(3) 0.047(3) -0.005(3) 0.000(3) -0.003(3)
C19 0.062(4) 0.055(3) 0.042(3) -0.017(3) -0.006(3) -0.007(3)
C20 0.036(3) 0.057(3) 0.050(3) -0.008(3) -0.011(2) -0.008(3)
C21 0.027(3) 0.046(3) 0.055(3) -0.007(2) -0.001(2) -0.011(2)
C22 0.032(3) 0.033(2) 0.041(3) 0.001(2) 0.001(2) -0.004(2)
C23 0.033(3) 0.057(3) 0.046(3) -0.007(3) 0.007(2) -0.005(2)
C24 0.053(4) 0.052(3) 0.047(3) -0.011(3) 0.010(3) 0.002(3)
C25 0.060(4) 0.044(3) 0.039(3) -0.011(2) 0.001(3) -0.009(3)
C26 0.042(3) 0.035(3) 0.040(3) -0.003(2) -0.004(2) -0.009(2)
C27 0.056(4) 0.056(3) 0.038(3) 0.002(3) -0.006(3) -0.008(3)
C28 0.048(3) 0.047(3) 0.047(3) 0.006(3) -0.007(3) 0.001(3)
C29 0.042(3) 0.039(3) 0.037(3) -0.002(2) 0.008(2) -0.003(2)
C30 0.057(4) 0.034(3) 0.050(3) -0.002(2) 0.008(3) -0.003(3)
C31 0.065(4) 0.031(3) 0.068(4) -0.005(3) 0.016(3) -0.012(3)
C32 0.044(3) 0.043(3) 0.095(5) -0.011(3) 0.008(3) -0.015(3)
C33 0.035(3) 0.036(3) 0.083(4) 0.000(3) 0.000(3) -0.008(2)
C35 0.039(3) 0.055(4) 0.085(5) -0.030(3) 0.022(3) -0.006(3)
O7 0.059(3) 0.064(3) 0.068(3) -0.006(2) 0.003(2) -0.004(2)
O8 0.039(2) 0.110(4) 0.070(3) -0.023(3) 0.015(2) -0.004(3)
O9 0.077(4) 0.101(4) 0.086(4) -0.021(3) -0.031(3) -0.029(3)
O10 0.077(3) 0.055(3) 0.084(3) -0.021(2) -0.001(3) -0.001(2)

_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 N1 2.041(5) . ?
Ni1 N5B 2.047(10) . ?
Ni1 N9 2.087(5) . ?
Ni1 N4 2.089(4) . ?
Ni1 N3 2.116(5) . ?
Ni1 N5A 2.165(9) . ?
Ni1 O1 2.286(4) . ?
Ni2 N2 2.077(4) . ?
Ni2 N11 2.085(5) . ?
Ni2 N7 2.088(4) . ?
Ni2 N8 2.142(4) . ?
Ni2 O2 2.172(4) . ?
Ni2 N6 2.173(5) . ?
Ni1 Ni2 4.5188(9) . ?
Cl1 O4B 1.362(8) . ?
Cl1 O4A 1.384(7) . ?
Cl1 O6A 1.393(7) . ?
Cl1 O6B 1.424(8) . ?
Cl1 O3A 1.450(6) . ?
Cl1 O3B 1.451(7) . ?
Cl1 O5B 1.474(8) . ?
Cl1 O5A 1.512(7) . ?
Cl2 O8 1.419(5) . ?
Cl2 O9 1.425(5) . ?
Cl2 O10 1.431(5) . ?
Cl2 O7 1.446(5) . ?
N1 C2 1.337(7) . ?
N1 N2 1.372(6) . ?
N2 C3 1.352(7) . ?
N3 C5 1.476(7) . ?
N3 C12B 1.480(10) . ?
N3 C4 1.492(8) . ?
N3 C12A 1.518(9) . ?
N4 C11 1.344(8) . ?
N4 C7 1.358(7) . ?
N6 C27 1.485(7) . ?
N6 C19 1.495(7) . ?
N6 C20 1.506(7) . ?
N7 C22 1.347(7) . ?
N7 C26 1.348(7) . ?
N8 C33 1.342(8) . ?
N8 C29 1.347(7) . ?
N9 N10 1.187(6) . ?
N10 N11 1.160(6) . ?
O1 C34B 1.399(10) . ?
O1 C34A 1.441(8) . ?
O2 C35 1.442(7) . ?
C1 C3 1.377(8) . ?
C1 C2 1.386(9) . ?
C2 C4 1.499(8) . ?
C3 C19 1.482(8) . ?
C5 C6 1.520(8) . ?
C6 C7 1.500(9) . ?
C7 C8 1.380(8) . ?
C8 C9 1.368(10) . ?
C9 C10 1.385(9) . ?
C10 C11 1.384(8) . ?
C12A C13A 1.512(15) . ?
C13A C14A 1.503(16) . ?
C14A N5A 1.369(11) . ?
C14A C15A 1.400(13) . ?
C15A C16A 1.371(17) . ?
C16A C17A 1.381(15) . ?
C17A C18A 1.362(10) . ?
C18A N5A 1.312(14) . ?
C12B C13B 1.495(16) . ?
C13B C14B 1.493(17) . ?
C14B N5B 1.369(12) . ?
C14B C15B 1.401(14) . ?
C15B C16B 1.366(17) . ?
C16B C17B 1.390(16) . ?
C17B C18B 1.364(11) . ?
C18B N5B 1.318(15) . ?
C20 C21 1.514(8) . ?
C21 C22 1.491(8) . ?
C22 C23 1.390(8) . ?
C23 C24 1.382(9) . ?
C24 C25 1.386(9) . ?
C25 C26 1.378(8) . ?
C27 C28 1.525(8) . ?
C28 C29 1.506(8) . ?
C29 C30 1.394(8) . ?
C30 C31 1.354(10) . ?
C31 C32 1.376(10) . ?
C32 C33 1.374(8) . ?

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
N1 Ni1 N5B 166.7(5) . . ?
N1 Ni1 N9 91.68(18) . . ?
N5B Ni1 N9 95.7(4) . . ?
N1 Ni1 N4 93.93(17) . . ?
N5B Ni1 N4 96.4(4) . . ?
N9 Ni1 N4 95.31(19) . . ?
N1 Ni1 N3 81.55(19) . . ?
N5B Ni1 N3 89.2(5) . . ?
N9 Ni1 N3 168.1(2) . . ?
N4 Ni1 N3 94.88(18) . . ?
N1 Ni1 N5A 172.7(3) . . ?
N5B Ni1 N5A 8.8(4) . . ?
N9 Ni1 N5A 87.7(4) . . ?
N4 Ni1 N5A 93.4(3) . . ?
N3 Ni1 N5A 97.7(4) . . ?
N1 Ni1 O1 85.49(17) . . ?
N5B Ni1 O1 84.2(4) . . ?
N9 Ni1 O1 85.03(19) . . ?
N4 Ni1 O1 179.34(18) . . ?
N3 Ni1 O1 84.72(17) . . ?
N5A Ni1 O1 87.2(3) . . ?
N2 Ni2 N11 94.58(17) . . ?
N2 Ni2 N7 104.04(15) . . ?
N11 Ni2 N7 90.18(18) . . ?
N2 Ni2 N8 164.55(16) . . ?
N11 Ni2 N8 91.64(18) . . ?
N7 Ni2 N8 90.05(16) . . ?
N2 Ni2 O2 84.26(16) . . ?
N11 Ni2 O2 87.4(2) . . ?
N7 Ni2 O2 171.53(16) . . ?
N8 Ni2 O2 81.91(16) . . ?
N2 Ni2 N6 79.71(18) . . ?
N11 Ni2 N6 174.26(17) . . ?
N7 Ni2 N6 91.79(16) . . ?
N8 Ni2 N6 93.75(17) . . ?
O2 Ni2 N6 91.39(19) . . ?
O4B Cl1 O4A 170.5(7) . . ?
O4B Cl1 O6A 72.2(6) . . ?
O4A Cl1 O6A 117.3(5) . . ?
O4B Cl1 O6B 114.7(6) . . ?
O6A Cl1 O6B 157.8(7) . . ?
O4A Cl1 O3A 111.2(5) . . ?
O6A Cl1 O3A 110.2(4) . . ?
O4B Cl1 O3B 114.4(5) . . ?
O6A Cl1 O3B 87.6(5) . . ?
O6B Cl1 O3B 106.7(5) . . ?
O3A Cl1 O3B 158.0(5) . . ?
O4B Cl1 O5B 109.8(5) . . ?
O4A Cl1 O5B 77.2(7) . . ?
O6B Cl1 O5B 106.8(5) . . ?
O3A Cl1 O5B 97.7(6) . . ?
O3B Cl1 O5B 103.5(5) . . ?
O4B Cl1 O5A 69.8(6) . . ?
O4A Cl1 O5A 106.6(5) . . ?
O6A Cl1 O5A 107.2(4) . . ?
O6B Cl1 O5A 94.9(7) . . ?
O3A Cl1 O5A 103.3(4) . . ?
O5B Cl1 O5A 155.3(6) . . ?
O8 Cl2 O9 110.0(3) . . ?
O8 Cl2 O10 109.9(3) . . ?
O9 Cl2 O10 109.7(3) . . ?
O8 Cl2 O7 109.6(3) . . ?
O9 Cl2 O7 108.9(3) . . ?
O10 Cl2 O7 108.8(3) . . ?
C2 N1 N2 107.5(5) . . ?
C2 N1 Ni1 113.6(4) . . ?
N2 N1 Ni1 138.8(3) . . ?
C3 N2 N1 107.2(4) . . ?
C3 N2 Ni2 111.7(4) . . ?
N1 N2 Ni2 140.9(3) . . ?
C5 N3 C12B 109.5(7) . . ?
C5 N3 C4 111.1(6) . . ?
C12B N3 C4 97.8(9) . . ?
C5 N3 C12A 106.1(6) . . ?
C4 N3 C12A 113.3(7) . . ?
C5 N3 Ni1 112.5(4) . . ?
C12B N3 Ni1 119.3(8) . . ?
C4 N3 Ni1 105.3(3) . . ?
C12A N3 Ni1 108.5(6) . . ?
C11 N4 C7 117.9(5) . . ?
C11 N4 Ni1 118.5(4) . . ?
C7 N4 Ni1 123.5(4) . . ?
C27 N6 C19 109.8(4) . . ?
C27 N6 C20 108.8(5) . . ?
C19 N6 C20 108.2(5) . . ?
C27 N6 Ni2 111.6(4) . . ?
C19 N6 Ni2 101.6(4) . . ?
C20 N6 Ni2 116.5(3) . . ?
C22 N7 C26 117.8(4) . . ?
C22 N7 Ni2 123.1(3) . . ?
C26 N7 Ni2 118.3(3) . . ?
C33 N8 C29 117.1(5) . . ?
C33 N8 Ni2 117.7(4) . . ?
C29 N8 Ni2 125.2(4) . . ?
N10 N9 Ni1 121.2(4) . . ?
N11 N10 N9 178.0(6) . . ?
N10 N11 Ni2 119.1(4) . . ?
C34B O1 Ni1 125.0(10) . . ?
C34A O1 Ni1 129.8(5) . . ?
C35 O2 Ni2 123.9(4) . . ?
C3 C1 C2 103.8(5) . . ?
N1 C2 C1 110.9(5) . . ?
N1 C2 C4 117.3(6) . . ?
C1 C2 C4 131.8(6) . . ?
N2 C3 C1 110.6(5) . . ?
N2 C3 C19 117.4(5) . . ?
C1 C3 C19 131.9(6) . . ?
N3 C4 C2 111.0(5) . . ?
N3 C5 C6 115.0(5) . . ?
C7 C6 C5 113.1(6) . . ?
N4 C7 C8 120.7(6) . . ?
N4 C7 C6 118.6(5) . . ?
C8 C7 C6 120.7(5) . . ?
C9 C8 C7 121.4(6) . . ?
C8 C9 C10 118.1(6) . . ?
C11 C10 C9 118.6(6) . . ?
N4 C11 C10 123.4(6) . . ?
C13A C12A N3 120.1(10) . . ?
C14A C13A C12A 117.0(8) . . ?
N5A C14A C15A 120.3(12) . . ?
N5A C14A C13A 120.4(9) . . ?
C15A C14A C13A 119.0(10) . . ?
C16A C15A C14A 118.5(10) . . ?
C15A C16A C17A 121.0(9) . . ?
C18A C17A C16A 116.4(13) . . ?
N5A C18A C17A 125.6(12) . . ?
C18A N5A C14A 118.1(9) . . ?
C18A N5A Ni1 117.6(7) . . ?
C14A N5A Ni1 123.2(9) . . ?
N3 C12B C13B 104.2(11) . . ?
C14B C13B C12B 119.7(10) . . ?
N5B C14B C15B 120.6(14) . . ?
N5B C14B C13B 121.4(10) . . ?
C15B C14B C13B 118.0(11) . . ?
C16B C15B C14B 120.1(12) . . ?
C15B C16B C17B 119.6(10) . . ?
C18B C17B C16B 115.7(14) . . ?
N5B C18B C17B 128.0(14) . . ?
C18B N5B C14B 115.8(10) . . ?
C18B N5B Ni1 116.6(8) . . ?
C14B N5B Ni1 127.6(10) . . ?
C3 C19 N6 108.7(4) . . ?
N6 C20 C21 115.5(4) . . ?
C22 C21 C20 112.9(4) . . ?
N7 C22 C23 121.5(5) . . ?
N7 C22 C21 117.4(4) . . ?
C23 C22 C21 121.1(5) . . ?
C24 C23 C22 120.1(5) . . ?
C23 C24 C25 118.3(5) . . ?
C26 C25 C24 118.6(5) . . ?
N7 C26 C25 123.5(5) . . ?
N6 C27 C28 111.6(5) . . ?
C29 C28 C27 114.3(5) . . ?
N8 C29 C30 121.1(6) . . ?
N8 C29 C28 118.5(5) . . ?
C30 C29 C28 120.4(5) . . ?
C31 C30 C29 120.5(6) . . ?
C30 C31 C32 119.2(5) . . ?
C33 C32 C31 117.8(6) . . ?
N8 C33 C32 124.4(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O3B 0.81(2) 2.16(4) 2.891(10) 149(4) 2_766
O1 H1 O5A 0.81(2) 2.43(4) 2.988(9) 127(3) 2_766
O2 H2 O6B 0.81(2) 1.84(6) 2.461(10) 133(7) .
O2 H2 O3A 0.81(2) 2.34(5) 3.022(9) 143(7) .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.086

#===END

data_2-nf18
_database_code_depnum_ccdc_archive 'CCDC 682092'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H37 N14 Ni2 +, N O3 -, C H4 O'
_chemical_formula_sum            'C34 H41 N15 Ni2 O4'
_chemical_formula_weight         841.24

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           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

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

_cell_length_a                   13.0038(4)
_cell_length_b                   16.9448(6)
_cell_length_c                   32.4543(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7151.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    70382
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      24.87

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3504
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_T_max  0.8375
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(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  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70382
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         24.87
_reflns_number_total             6173
_reflns_number_gt                4742
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (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^)+(0.0711P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6173
_refine_ls_number_parameters     493
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1074
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_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
Ni1 Ni 0.84767(3) 0.20643(2) 0.603096(12) 0.03133(12) Uani 1 1 d . . .
Ni2 Ni 0.51494(3) 0.24909(2) 0.563351(12) 0.03130(12) Uani 1 1 d . . .
O1A O 0.2603(5) 0.0842(3) 0.7061(2) 0.0617(19) Uiso 0.630(13) 1 d PD A 1
O2A O 0.2658(5) -0.0405(3) 0.71788(15) 0.075(2) Uiso 0.630(13) 1 d PD A 1
O3A O 0.2140(5) 0.0030(3) 0.65852(12) 0.0546(16) Uiso 0.630(13) 1 d PD A 1
O1B O 0.1962(10) -0.0428(5) 0.7128(3) 0.095(4) Uiso 0.370(13) 1 d PD A 2
O2B O 0.2434(12) 0.0150(7) 0.6573(2) 0.110(5) Uiso 0.370(13) 1 d PD A 2
O3B O 0.2540(9) 0.0762(4) 0.7164(3) 0.062(3) Uiso 0.370(13) 1 d PD A 2
N1 N 0.71878(18) 0.14582(13) 0.58080(8) 0.0320(6) Uani 1 1 d . . .
N2 N 0.62050(18) 0.15868(14) 0.56686(8) 0.0314(5) Uani 1 1 d . . .
N3 N 0.87588(19) 0.09155(14) 0.62801(8) 0.0367(6) Uani 1 1 d . . .
N4 N 0.7804(2) 0.24689(14) 0.65810(8) 0.0376(6) Uani 1 1 d . . .
N5 N 0.99232(18) 0.25620(14) 0.62328(8) 0.0346(6) Uani 1 1 d . . .
N6 N 0.40930(18) 0.15116(14) 0.56078(8) 0.0328(6) Uani 1 1 d . . .
N7 N 0.49284(19) 0.26143(15) 0.62787(9) 0.0374(6) Uani 1 1 d . . .
N8 N 0.40246(19) 0.33811(14) 0.55124(8) 0.0342(6) Uani 1 1 d . . .
N9 N 0.80857(19) 0.31104(14) 0.57221(8) 0.0345(6) Uani 1 1 d . . .
N11 N 0.6320(2) 0.33505(15) 0.56320(10) 0.0435(7) Uani 1 1 d . . .
N10 N 0.7198(2) 0.32184(13) 0.56777(8) 0.0319(6) Uani 1 1 d . . .
N12 N 0.52434(19) 0.24246(15) 0.49628(9) 0.0370(6) Uani 1 1 d . . .
N13 N 0.48015(19) 0.28458(15) 0.47333(9) 0.0344(6) Uani 1 1 d . . .
N14 N 0.4372(2) 0.32729(15) 0.45011(9) 0.0372(6) Uani 1 1 d . . .
N15 N 0.2407(2) 0.01456(16) 0.69524(10) 0.0566(8) Uani 1 1 d D . .
C1 C 0.6478(2) 0.02756(17) 0.56639(10) 0.0357(7) Uani 1 1 d . . .
H1 H 0.6382 -0.0265 0.5634 0.080 Uiso 1 1 calc R . .
C3 C 0.5791(2) 0.08805(17) 0.55782(10) 0.0339(7) Uani 1 1 d . . .
C2 C 0.7348(2) 0.06731(17) 0.58045(10) 0.0347(7) Uani 1 1 d . . .
C4 C 0.8380(2) 0.03910(17) 0.59425(11) 0.0385(7) Uani 1 1 d . . .
H4B H 0.8859 0.0402 0.5713 0.080 Uiso 1 1 calc R . .
H4A H 0.8330 -0.0148 0.6041 0.080 Uiso 1 1 calc R . .
C5 C 0.8214(3) 0.0704(2) 0.66742(12) 0.0485(9) Uani 1 1 d . . .
H5B H 0.8681 0.0799 0.6902 0.080 Uiso 1 1 calc R . .
H5A H 0.8067 0.0143 0.6669 0.080 Uiso 1 1 calc R . .
C6 C 0.7219(3) 0.1140(2) 0.67598(11) 0.0451(8) Uani 1 1 d . . .
H6A H 0.6779 0.1101 0.6519 0.080 Uiso 1 1 calc R . .
H6B H 0.6869 0.0884 0.6987 0.080 Uiso 1 1 calc R . .
C7 C 0.7366(3) 0.1994(2) 0.68630(10) 0.0415(8) Uani 1 1 d . . .
C8 C 0.7055(4) 0.2282(2) 0.72436(12) 0.0596(10) Uani 1 1 d . . .
H8 H 0.6770 0.1943 0.7438 0.080 Uiso 1 1 calc R . .
C9 C 0.7171(4) 0.3070(2) 0.73328(13) 0.0717(13) Uani 1 1 d . . .
H9 H 0.6956 0.3270 0.7585 0.080 Uiso 1 1 calc R . .
C10 C 0.7608(3) 0.3561(2) 0.70436(11) 0.0558(10) Uani 1 1 d . . .
H10 H 0.7693 0.4097 0.7096 0.080 Uiso 1 1 calc R . .
C11 C 0.7915(3) 0.32397(19) 0.66761(10) 0.0415(8) Uani 1 1 d . . .
H11 H 0.8216 0.3571 0.6482 0.080 Uiso 1 1 calc R . .
C12 C 0.9877(2) 0.07918(19) 0.63411(13) 0.0459(8) Uani 1 1 d . . .
H12A H 1.0223 0.0838 0.6077 0.080 Uiso 1 1 calc R . .
H12B H 0.9990 0.0261 0.6443 0.080 Uiso 1 1 calc R . .
C13 C 1.0350(3) 0.1381(2) 0.66427(13) 0.0528(10) Uani 1 1 d . . .
H13A H 0.9878 0.1448 0.6872 0.080 Uiso 1 1 calc R . .
H13B H 1.0977 0.1152 0.6752 0.080 Uiso 1 1 calc R . .
C14 C 1.0603(2) 0.21848(18) 0.64754(10) 0.0362(7) Uani 1 1 d . . .
C15 C 1.1528(2) 0.25312(18) 0.65907(11) 0.0387(7) Uani 1 1 d . . .
H15 H 1.1989 0.2254 0.6755 0.080 Uiso 1 1 calc R . .
C16 C 1.1766(3) 0.3284(2) 0.64622(11) 0.0443(8) Uani 1 1 d . . .
H16 H 1.2375 0.3526 0.6543 0.080 Uiso 1 1 calc R . .
C17 C 1.1069(3) 0.36710(19) 0.62091(11) 0.0420(8) Uani 1 1 d . . .
H17 H 1.1203 0.4180 0.6116 0.080 Uiso 1 1 calc R . .
C18 C 1.0183(2) 0.32913(18) 0.60986(10) 0.0379(7) Uani 1 1 d . . .
H18 H 0.9734 0.3549 0.5921 0.080 Uiso 1 1 calc R . .
C19 C 0.4718(2) 0.08794(17) 0.54092(11) 0.0363(7) Uani 1 1 d . . .
H19A H 0.4739 0.0965 0.5114 0.080 Uiso 1 1 calc R . .
H19B H 0.4401 0.0370 0.5459 0.080 Uiso 1 1 calc R . .
C20 C 0.3687(2) 0.12178(19) 0.60082(10) 0.0393(7) Uani 1 1 d . . .
H20A H 0.3447 0.0681 0.5970 0.080 Uiso 1 1 calc R . .
H20B H 0.3096 0.1536 0.6084 0.080 Uiso 1 1 calc R . .
C21 C 0.4445(3) 0.12270(18) 0.63647(11) 0.0401(7) Uani 1 1 d . . .
H21A H 0.4190 0.0887 0.6582 0.080 Uiso 1 1 calc R . .
H21B H 0.5098 0.1015 0.6271 0.080 Uiso 1 1 calc R . .
C22 C 0.4614(2) 0.20373(19) 0.65345(11) 0.0396(7) Uani 1 1 d . . .
C23 C 0.4397(3) 0.2191(2) 0.69445(12) 0.0569(10) Uani 1 1 d . . .
H23 H 0.4179 0.1786 0.7117 0.080 Uiso 1 1 calc R . .
C24 C 0.4503(4) 0.2946(3) 0.70956(13) 0.0730(13) Uani 1 1 d . . .
H24 H 0.4346 0.3058 0.7369 0.080 Uiso 1 1 calc R . .
C25 C 0.4845(4) 0.3535(2) 0.68362(12) 0.0625(11) Uani 1 1 d . . .
H25 H 0.4941 0.4046 0.6933 0.080 Uiso 1 1 calc R . .
C26 C 0.5040(3) 0.3352(2) 0.64349(11) 0.0460(8) Uani 1 1 d . . .
H26 H 0.5260 0.3753 0.6260 0.080 Uiso 1 1 calc R . .
C27 C 0.3205(2) 0.17069(18) 0.53347(11) 0.0388(7) Uani 1 1 d . . .
H27A H 0.2750 0.1254 0.5323 0.080 Uiso 1 1 calc R . .
H27B H 0.3461 0.1802 0.5058 0.080 Uiso 1 1 calc R . .
C28 C 0.2588(2) 0.24213(18) 0.54720(12) 0.0416(8) Uani 1 1 d . . .
H28A H 0.1932 0.2405 0.5330 0.080 Uiso 1 1 calc R . .
H28B H 0.2447 0.2361 0.5764 0.080 Uiso 1 1 calc R . .
C29 C 0.3039(2) 0.32339(18) 0.54084(10) 0.0346(7) Uani 1 1 d . . .
C30 C 0.2403(2) 0.38174(18) 0.52534(10) 0.0395(7) Uani 1 1 d . . .
H30 H 0.1732 0.3696 0.5177 0.080 Uiso 1 1 calc R . .
C31 C 0.2763(2) 0.45819(18) 0.52113(11) 0.0403(8) Uani 1 1 d . . .
H31 H 0.2339 0.4979 0.5111 0.080 Uiso 1 1 calc R . .
C32 C 0.3769(3) 0.47401(19) 0.53224(11) 0.0422(8) Uani 1 1 d . . .
H32 H 0.4034 0.5248 0.5302 0.080 Uiso 1 1 calc R . .
C33 C 0.4364(2) 0.41323(18) 0.54636(11) 0.0389(7) Uani 1 1 d . . .
H33 H 0.5045 0.4241 0.5530 0.080 Uiso 1 1 calc R . .
O4A O 0.4844(15) -0.0308(8) 0.7239(5) 0.109(7) Uiso 0.295(12) 1 d PD B 3
H4C H 0.4217 -0.0353 0.7252 0.080 Uiso 0.295(12) 1 calc PR B 3
C34A C 0.5153(14) 0.0370(8) 0.7460(5) 0.060(4) Uiso 0.295(12) 1 d PD B 3
H34A H 0.5290 0.0228 0.7741 0.080 Uiso 0.295(12) 1 calc PR B 3
H34B H 0.4614 0.0757 0.7451 0.080 Uiso 0.295(12) 1 calc PR B 3
H34C H 0.5764 0.0584 0.7338 0.080 Uiso 0.295(12) 1 calc PR B 3
O4B O 0.4549(5) 0.0214(3) 0.75221(15) 0.081(2) Uiso 0.705(12) 1 d PD B 4
H4D H 0.4130 0.0460 0.7384 0.080 Uiso 0.705(12) 1 calc PR B 4
C34B C 0.5216(7) -0.0200(5) 0.7259(2) 0.074(2) Uiso 0.705(12) 1 d PD B 4
H34D H 0.5877 0.0053 0.7256 0.080 Uiso 0.705(12) 1 calc PR B 4
H34E H 0.4938 -0.0203 0.6985 0.080 Uiso 0.705(12) 1 calc PR B 4
H34F H 0.5290 -0.0733 0.7355 0.080 Uiso 0.705(12) 1 calc PR B 4

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 0.0300(2) 0.02452(19) 0.0395(2) 0.00155(16) -0.00184(16) -0.00073(15)
Ni2 0.0278(2) 0.0243(2) 0.0418(2) -0.00160(16) -0.00018(16) -0.00048(15)
N1 0.0309(13) 0.0224(12) 0.0428(15) 0.0014(10) -0.0004(11) 0.0012(10)
N2 0.0277(12) 0.0260(12) 0.0404(14) -0.0026(11) 0.0001(11) -0.0022(10)
N3 0.0323(13) 0.0290(13) 0.0487(16) 0.0038(11) -0.0016(12) -0.0012(10)
N4 0.0362(14) 0.0365(14) 0.0400(15) 0.0013(12) -0.0034(12) 0.0007(11)
N5 0.0331(13) 0.0297(13) 0.0410(15) 0.0017(11) -0.0019(11) 0.0004(11)
N6 0.0283(13) 0.0274(12) 0.0429(15) -0.0009(11) 0.0000(11) -0.0003(10)
N7 0.0341(14) 0.0323(13) 0.0460(16) -0.0012(12) -0.0020(12) 0.0000(11)
N8 0.0321(13) 0.0293(13) 0.0412(15) -0.0050(11) -0.0002(11) 0.0014(11)
N9 0.0286(14) 0.0282(12) 0.0466(16) 0.0026(11) -0.0035(11) -0.0019(10)
N11 0.0312(15) 0.0268(13) 0.072(2) 0.0025(13) -0.0031(13) 0.0009(11)
N10 0.0388(17) 0.0214(12) 0.0355(14) -0.0022(10) -0.0013(11) -0.0036(11)
N12 0.0313(13) 0.0364(14) 0.0432(16) 0.0004(12) 0.0000(12) 0.0049(11)
N13 0.0267(13) 0.0309(13) 0.0456(16) -0.0061(13) 0.0064(12) -0.0038(11)
N14 0.0362(14) 0.0306(13) 0.0450(16) 0.0025(12) -0.0031(12) 0.0021(12)
N15 0.060(2) 0.0375(16) 0.072(2) 0.0118(16) 0.0130(17) 0.0079(14)
C1 0.0329(16) 0.0225(14) 0.052(2) -0.0049(13) 0.0013(14) -0.0008(12)
C3 0.0306(15) 0.0274(14) 0.0439(18) -0.0020(13) 0.0029(13) -0.0039(12)
C2 0.0340(16) 0.0254(14) 0.0447(18) 0.0014(13) 0.0006(14) 0.0018(12)
C4 0.0341(16) 0.0260(14) 0.055(2) -0.0010(14) -0.0030(14) 0.0013(13)
C5 0.056(2) 0.0358(17) 0.054(2) 0.0140(16) 0.0029(17) -0.0005(16)
C6 0.048(2) 0.0431(18) 0.0438(19) 0.0044(15) 0.0041(16) -0.0075(16)
C7 0.0392(18) 0.0453(19) 0.0401(19) 0.0046(15) -0.0030(15) 0.0067(15)
C8 0.082(3) 0.053(2) 0.044(2) 0.0104(18) 0.008(2) 0.010(2)
C9 0.118(4) 0.056(2) 0.040(2) 0.0018(18) 0.012(2) 0.022(3)
C10 0.084(3) 0.043(2) 0.040(2) -0.0017(16) -0.004(2) 0.0158(19)
C11 0.0450(19) 0.0373(17) 0.0421(19) 0.0011(14) -0.0055(15) 0.0064(14)
C12 0.0389(18) 0.0313(16) 0.067(2) 0.0065(16) -0.0137(17) 0.0034(14)
C13 0.054(2) 0.0400(19) 0.064(2) 0.0155(17) -0.0221(19) -0.0092(16)
C14 0.0369(17) 0.0339(15) 0.0379(18) 0.0011(13) -0.0013(13) -0.0009(13)
C15 0.0366(16) 0.0388(17) 0.0407(18) 0.0002(14) -0.0041(14) 0.0002(14)
C16 0.0374(17) 0.0468(19) 0.049(2) -0.0052(16) -0.0058(14) -0.0051(15)
C17 0.0435(18) 0.0333(16) 0.049(2) -0.0003(14) -0.0024(16) -0.0065(14)
C18 0.0368(16) 0.0318(16) 0.0451(19) 0.0007(14) -0.0011(14) -0.0018(13)
C19 0.0314(16) 0.0288(15) 0.0486(19) -0.0084(13) -0.0023(14) 0.0001(12)
C20 0.0346(17) 0.0319(15) 0.051(2) 0.0006(14) 0.0032(15) -0.0060(13)
C21 0.0422(18) 0.0341(16) 0.0442(19) 0.0060(14) 0.0044(15) -0.0013(14)
C22 0.0348(17) 0.0398(18) 0.0441(19) 0.0003(15) -0.0039(14) -0.0022(13)
C23 0.067(3) 0.061(2) 0.043(2) 0.0021(18) 0.0010(18) -0.015(2)
C24 0.108(4) 0.065(3) 0.046(2) -0.017(2) 0.010(2) -0.024(3)
C25 0.090(3) 0.048(2) 0.050(2) -0.0161(18) 0.003(2) -0.011(2)
C26 0.051(2) 0.0380(18) 0.049(2) -0.0052(16) -0.0027(16) -0.0043(15)
C27 0.0296(16) 0.0344(16) 0.052(2) -0.0023(15) -0.0060(14) -0.0032(13)
C28 0.0266(15) 0.0347(17) 0.063(2) 0.0020(16) -0.0044(15) -0.0024(13)
C29 0.0288(15) 0.0328(15) 0.0423(18) -0.0051(13) 0.0003(13) 0.0019(12)
C30 0.0322(16) 0.0372(17) 0.049(2) -0.0085(15) -0.0010(14) 0.0039(13)
C31 0.0382(17) 0.0329(16) 0.050(2) -0.0102(14) -0.0045(15) 0.0105(14)
C32 0.0396(18) 0.0295(16) 0.057(2) -0.0049(14) -0.0017(16) 0.0020(13)
C33 0.0317(16) 0.0313(16) 0.054(2) -0.0052(14) -0.0018(15) -0.0001(13)

_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 N1 2.095(2) . ?
Ni1 N9 2.099(2) . ?
Ni1 N4 2.103(3) . ?
Ni1 N3 2.139(2) . ?
Ni1 N14 2.160(3) 4_556 ?
Ni1 N5 2.163(2) . ?
Ni2 N2 2.060(2) . ?
Ni2 N11 2.107(3) . ?
Ni2 N7 2.124(3) . ?
Ni2 N8 2.138(2) . ?
Ni2 N6 2.156(2) . ?
Ni2 N12 2.183(3) . ?
Ni1 Ni2 4.5725(5) . ?
Ni1 Ni2 5.8720(6) 4_556 ?
O1A N15 1.258(5) . ?
O2A N15 1.231(4) . ?
O3A N15 1.256(4) . ?
O1B N15 1.266(6) . ?
O2B N15 1.232(6) . ?
O3B N15 1.262(5) . ?
N1 C2 1.347(4) . ?
N1 N2 1.373(3) . ?
N2 C3 1.345(4) . ?
N3 C12 1.482(4) . ?
N3 C4 1.494(4) . ?
N3 C5 1.505(4) . ?
N4 C7 1.345(4) . ?
N4 C11 1.350(4) . ?
N5 C14 1.346(4) . ?
N5 C18 1.353(4) . ?
N6 C20 1.489(4) . ?
N6 C19 1.491(4) . ?
N6 C27 1.493(4) . ?
N7 C22 1.346(4) . ?
N7 C26 1.357(4) . ?
N8 C29 1.349(4) . ?
N8 C33 1.357(4) . ?
N9 N10 1.178(4) . ?
N11 N10 1.173(4) . ?
N12 N13 1.181(4) . ?
N13 N14 1.184(4) . ?
N14 Ni1 2.160(3) 4_456 ?
C1 C3 1.388(4) . ?
C1 C2 1.393(4) . ?
C3 C19 1.499(4) . ?
C2 C4 1.494(4) . ?
C5 C6 1.516(5) . ?
C6 C7 1.497(5) . ?
C7 C8 1.388(5) . ?
C8 C9 1.375(6) . ?
C9 C10 1.377(6) . ?
C10 C11 1.370(5) . ?
C12 C13 1.528(5) . ?
C13 C14 1.502(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.377(5) . ?
C16 C17 1.388(5) . ?
C17 C18 1.367(4) . ?
C20 C21 1.520(5) . ?
C21 C22 1.496(4) . ?
C22 C23 1.385(5) . ?
C23 C24 1.377(6) . ?
C24 C25 1.379(6) . ?
C25 C26 1.362(5) . ?
C27 C28 1.519(4) . ?
C28 C29 1.510(4) . ?
C29 C30 1.383(4) . ?
C30 C31 1.384(5) . ?
C31 C32 1.382(5) . ?
C32 C33 1.368(4) . ?
O4A C34A 1.412(10) . ?
O4B C34B 1.406(7) . ?

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
N1 Ni1 N9 93.17(9) . . ?
N1 Ni1 N4 96.91(10) . . ?
N9 Ni1 N4 91.68(10) . . ?
N1 Ni1 N3 79.73(9) . . ?
N9 Ni1 N3 172.06(10) . . ?
N4 Ni1 N3 92.70(10) . . ?
N1 Ni1 N14 91.47(10) . 4_556 ?
N9 Ni1 N14 88.41(10) . 4_556 ?
N4 Ni1 N14 171.60(10) . 4_556 ?
N3 Ni1 N14 88.22(10) . 4_556 ?
N1 Ni1 N5 172.59(9) . . ?
N9 Ni1 N5 91.49(10) . . ?
N4 Ni1 N5 88.71(10) . . ?
N3 Ni1 N5 95.23(9) . . ?
N14 Ni1 N5 82.89(10) 4_556 . ?
N2 Ni2 N11 91.88(10) . . ?
N2 Ni2 N7 96.25(10) . . ?
N11 Ni2 N7 91.83(11) . . ?
N2 Ni2 N8 172.25(10) . . ?
N11 Ni2 N8 90.34(10) . . ?
N7 Ni2 N8 91.10(10) . . ?
N2 Ni2 N6 81.63(9) . . ?
N11 Ni2 N6 172.96(10) . . ?
N7 Ni2 N6 91.59(10) . . ?
N8 Ni2 N6 95.74(9) . . ?
N2 Ni2 N12 88.83(10) . . ?
N11 Ni2 N12 89.59(11) . . ?
N7 Ni2 N12 174.67(10) . . ?
N8 Ni2 N12 83.75(10) . . ?
N6 Ni2 N12 87.57(10) . . ?
C2 N1 N2 107.3(2) . . ?
C2 N1 Ni1 111.32(19) . . ?
N2 N1 Ni1 141.34(18) . . ?
C3 N2 N1 107.6(2) . . ?
C3 N2 Ni2 112.5(2) . . ?
N1 N2 Ni2 139.14(18) . . ?
C12 N3 C4 109.7(3) . . ?
C12 N3 C5 108.3(3) . . ?
C4 N3 C5 109.0(2) . . ?
C12 N3 Ni1 110.33(19) . . ?
C4 N3 Ni1 101.98(18) . . ?
C5 N3 Ni1 117.21(19) . . ?
C7 N4 C11 117.9(3) . . ?
C7 N4 Ni1 124.0(2) . . ?
C11 N4 Ni1 117.7(2) . . ?
C14 N5 C18 117.2(3) . . ?
C14 N5 Ni1 124.3(2) . . ?
C18 N5 Ni1 118.4(2) . . ?
C20 N6 C19 109.3(2) . . ?
C20 N6 C27 108.5(2) . . ?
C19 N6 C27 108.9(2) . . ?
C20 N6 Ni2 116.74(19) . . ?
C19 N6 Ni2 102.84(17) . . ?
C27 N6 Ni2 110.20(18) . . ?
C22 N7 C26 118.1(3) . . ?
C22 N7 Ni2 125.3(2) . . ?
C26 N7 Ni2 116.4(2) . . ?
C29 N8 C33 117.0(3) . . ?
C29 N8 Ni2 124.5(2) . . ?
C33 N8 Ni2 117.4(2) . . ?
N10 N9 Ni1 115.3(2) . . ?
N10 N11 Ni2 124.8(2) . . ?
N11 N10 N9 177.9(3) . . ?
N13 N12 Ni2 124.8(2) . . ?
N12 N13 N14 179.0(3) . . ?
N13 N14 Ni1 126.9(2) . 4_456 ?
O2A N15 O2B 126.4(7) . . ?
O2A N15 O3A 121.4(4) . . ?
O2A N15 O1A 119.3(4) . . ?
O2B N15 O1A 105.5(6) . . ?
O3A N15 O1A 117.8(4) . . ?
O2A N15 O3B 105.4(6) . . ?
O2B N15 O3B 122.3(6) . . ?
O3A N15 O3B 133.0(6) . . ?
O2B N15 O1B 117.9(6) . . ?
O3A N15 O1B 100.5(6) . . ?
O1A N15 O1B 133.4(6) . . ?
O3B N15 O1B 116.9(5) . . ?
C3 C1 C2 103.4(3) . . ?
N2 C3 C1 110.9(3) . . ?
N2 C3 C19 116.9(3) . . ?
C1 C3 C19 132.2(3) . . ?
N1 C2 C1 110.8(3) . . ?
N1 C2 C4 116.9(3) . . ?
C1 C2 C4 132.3(3) . . ?
C2 C4 N3 109.0(2) . . ?
N3 C5 C6 116.2(3) . . ?
C7 C6 C5 113.9(3) . . ?
N4 C7 C8 121.2(3) . . ?
N4 C7 C6 118.7(3) . . ?
C8 C7 C6 120.1(3) . . ?
C9 C8 C7 119.8(4) . . ?
C8 C9 C10 119.2(4) . . ?
C11 C10 C9 118.3(4) . . ?
N4 C11 C10 123.5(3) . . ?
N3 C12 C13 112.8(3) . . ?
C14 C13 C12 116.7(3) . . ?
N5 C14 C15 121.7(3) . . ?
N5 C14 C13 119.9(3) . . ?
C15 C14 C13 118.4(3) . . ?
C16 C15 C14 120.3(3) . . ?
C15 C16 C17 118.1(3) . . ?
C18 C17 C16 118.9(3) . . ?
N5 C18 C17 123.8(3) . . ?
N6 C19 C3 110.4(2) . . ?
N6 C20 C21 115.5(3) . . ?
C22 C21 C20 112.7(3) . . ?
N7 C22 C23 121.2(3) . . ?
N7 C22 C21 118.9(3) . . ?
C23 C22 C21 119.8(3) . . ?
C24 C23 C22 119.8(4) . . ?
C23 C24 C25 119.1(4) . . ?
C26 C25 C24 118.7(4) . . ?
N7 C26 C25 123.1(3) . . ?
N6 C27 C28 114.3(3) . . ?
C29 C28 C27 118.8(3) . . ?
N8 C29 C30 121.8(3) . . ?
N8 C29 C28 120.2(3) . . ?
C30 C29 C28 118.0(3) . . ?
C29 C30 C31 120.2(3) . . ?
C32 C31 C30 118.4(3) . . ?
C33 C32 C31 118.5(3) . . ?
N8 C33 C32 124.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.87
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.064

# start Validation Reply Form

_vrf_PLAT027_1-k138-1            
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 24.68 Deg.
RESPONSE: Unfortunately this cannot be changed now. Theta max is, however,
close to 25.00 deg.
;
_vrf_PLAT410_1-k138-1            
;
PROBLEM: Short Intra H...H Contact H5A .. H13C .. 1.70 Ang.
RESPONSE: One of the calculated H-atoms of the disorderd part (H13C)
comes close to an calculated H-atom (H5A) of the non-disordered part.
A disorder of the H-atoms of the non-disordered part can be assumed.
A refinement of the latter, however, would result in more restraints
and would not markedly improve the overall quality of the
structure determination.
;
_vrf_PLAT027_2-nf18              
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 24.68 Deg.
RESPONSE: Unfortunately this cannot be changed now. Theta max is, however,
close to 25.00 deg.
;

# end Validation Reply Form