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#$Date: 2016-03-21 06:27:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178511 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/14/4061458.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4061458
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om0501780
_journal_year                    2005
_chemical_formula_sum            'C67 H91 Cl3 N6 Ni2 O10'
_chemical_formula_weight         1364.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.239(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.606(4)
_cell_length_b                   15.396(3)
_cell_length_c                   26.072(6)
_cell_measurement_temperature    117(1)
_cell_volume                     7170(3)
_diffrn_ambient_temperature      117(1)
_exptl_crystal_density_diffrn    1.264
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4061458
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
C1A C 0.1267(4) 0.2495(4) 0.2441(3) 0.0447(18) Uani 1 1 d . . .
C2A C 0.0747(5) 0.2272(5) 0.1958(3) 0.057(2) Uani 1 1 d . . .
H2A H 0.0238 0.2327 0.1925 0.069 Uiso 1 1 calc R . .
C3A C 0.0972(5) 0.1978(5) 0.1535(3) 0.054(2) Uani 1 1 d . . .
H3A H 0.0614 0.1828 0.1221 0.065 Uiso 1 1 calc R . .
C4A C 0.1726(5) 0.1898(4) 0.1564(3) 0.0469(19) Uani 1 1 d . . .
H4A H 0.1870 0.1691 0.1272 0.056 Uiso 1 1 calc R . .
C5A C 0.2264(4) 0.2129(4) 0.2032(3) 0.0394(17) Uani 1 1 d . . .
C6A C 0.2019(4) 0.2442(4) 0.2460(3) 0.0345(16) Uani 1 1 d . . .
C7A C 0.2818(4) 0.3469(4) 0.3041(3) 0.0409(17) Uani 1 1 d . . .
C8A C 0.3362(4) 0.3571(4) 0.3584(3) 0.0384(17) Uani 1 1 d . . .
C9A C 0.3757(4) 0.4296(4) 0.3810(3) 0.0448(19) Uani 1 1 d . . .
H9A H 0.3712 0.4813 0.3619 0.054 Uiso 1 1 calc R . .
C10A C 0.4214(4) 0.4245(4) 0.4316(3) 0.0426(18) Uani 1 1 d . . .
H10A H 0.4485 0.4731 0.4471 0.051 Uiso 1 1 calc R . .
C11A C 0.4284(4) 0.3481(4) 0.4606(3) 0.0409(17) Uani 1 1 d . . .
H11A H 0.4590 0.3449 0.4955 0.049 Uiso 1 1 calc R . .
C12A C 0.3886(4) 0.2770(4) 0.4360(2) 0.0287(14) Uani 1 1 d . . .
C13A C 0.3870(4) 0.1862(4) 0.4576(3) 0.0326(15) Uani 1 1 d . . .
C14A C 0.3396(4) 0.0442(4) 0.4331(2) 0.0352(16) Uani 1 1 d . . .
C15A C 0.2849(4) 0.0132(4) 0.4564(3) 0.0449(18) Uani 1 1 d . . .
C16A C 0.2849(5) -0.0773(5) 0.4662(3) 0.059(2) Uani 1 1 d . . .
H16A H 0.2494 -0.1006 0.4813 0.071 Uiso 1 1 calc R . .
C17A C 0.3353(5) -0.1300(4) 0.4541(3) 0.054(2) Uani 1 1 d . . .
H17A H 0.3347 -0.1890 0.4617 0.065 Uiso 1 1 calc R . .
C18A C 0.3876(5) -0.0991(4) 0.4309(3) 0.054(2) Uani 1 1 d . . .
H18A H 0.4215 -0.1374 0.4228 0.065 Uiso 1 1 calc R . .
C19A C 0.3910(4) -0.0098(4) 0.4188(3) 0.0417(18) Uani 1 1 d . . .
C20A C 0.0995(5) 0.2824(6) 0.2894(3) 0.061(2) Uani 1 1 d . . .
H20A H 0.142(5) 0.275(5) 0.321(3) 0.073 Uiso 1 1 calc . . .
C21A C 0.0364(6) 0.2327(7) 0.2996(5) 0.109(4) Uani 1 1 d . . .
H21A H -0.0083 0.2429 0.2711 0.164 Uiso 1 1 calc R . .
H21B H 0.0286 0.2514 0.3328 0.164 Uiso 1 1 calc R . .
H21C H 0.0480 0.1719 0.3016 0.164 Uiso 1 1 calc R . .
C22A C 0.0824(8) 0.3764(6) 0.2868(5) 0.115(4) Uani 1 1 d . . .
H22A H 0.1128 0.4058 0.2679 0.173 Uiso 1 1 calc R . .
H22B H 0.0928 0.3994 0.3224 0.173 Uiso 1 1 calc R . .
H22C H 0.0305 0.3852 0.2684 0.173 Uiso 1 1 calc R . .
C23A C 0.3084(4) 0.2058(4) 0.2064(3) 0.0461(19) Uani 1 1 d . . .
H23A H 0.333(4) 0.253(5) 0.230(3) 0.055 Uiso 1 1 calc . . .
C24A C 0.3436(6) 0.1226(6) 0.2329(4) 0.079(3) Uani 1 1 d . . .
H24A H 0.3167 0.0737 0.2140 0.119 Uiso 1 1 calc R . .
H24B H 0.3416 0.1216 0.2693 0.119 Uiso 1 1 calc R . .
H24C H 0.3949 0.1199 0.2321 0.119 Uiso 1 1 calc R . .
C25A C 0.3275(5) 0.2172(5) 0.1542(3) 0.062(2) Uani 1 1 d . . .
H25A H 0.3034 0.1725 0.1297 0.093 Uiso 1 1 calc R . .
H25B H 0.3807 0.2133 0.1603 0.093 Uiso 1 1 calc R . .
H25C H 0.3104 0.2731 0.1393 0.093 Uiso 1 1 calc R . .
C26A C 0.2294(6) 0.0723(6) 0.4710(4) 0.074(3) Uani 1 1 d . . .
H26A H 0.250(5) 0.131(6) 0.473(3) 0.089 Uiso 1 1 calc . . .
C27A C 0.1548(8) 0.0723(10) 0.4276(4) 0.138(6) Uani 1 1 d . . .
H27A H 0.1622 0.0940 0.3949 0.207 Uiso 1 1 calc R . .
H27B H 0.1198 0.1088 0.4384 0.207 Uiso 1 1 calc R . .
H27C H 0.1356 0.0141 0.4221 0.207 Uiso 1 1 calc R . .
C28A C 0.2156(6) 0.0519(7) 0.5245(4) 0.092(3) Uani 1 1 d . . .
H28A H 0.1830 0.0026 0.5208 0.139 Uiso 1 1 calc R . .
H28B H 0.1927 0.1011 0.5362 0.139 Uiso 1 1 calc R . .
H28C H 0.2624 0.0392 0.5504 0.139 Uiso 1 1 calc R . .
C29A C 0.4467(4) 0.0224(4) 0.3915(3) 0.0402(18) Uani 1 1 d . . .
H29A H 0.429(4) 0.079(4) 0.376(3) 0.048 Uiso 1 1 calc . . .
C30A C 0.5221(4) 0.0379(5) 0.4321(3) 0.054(2) Uani 1 1 d . . .
H30A H 0.5155 0.0754 0.4599 0.081 Uiso 1 1 calc R . .
H30B H 0.5556 0.0648 0.4148 0.081 Uiso 1 1 calc R . .
H30C H 0.5427 -0.0165 0.4473 0.081 Uiso 1 1 calc R . .
C31A C 0.4543(5) -0.0335(6) 0.3465(3) 0.068(2) Uani 1 1 d . . .
H31A H 0.4729 -0.0896 0.3600 0.102 Uiso 1 1 calc R . .
H31B H 0.4886 -0.0069 0.3298 0.102 Uiso 1 1 calc R . .
H31C H 0.4063 -0.0399 0.3208 0.102 Uiso 1 1 calc R . .
C1B C 0.4752(4) 0.6072(4) 0.6939(3) 0.0404(17) Uani 1 1 d . . .
C2B C 0.5038(4) 0.6914(4) 0.6956(3) 0.0500(19) Uani 1 1 d . . .
H2B H 0.5392 0.7109 0.7262 0.060 Uiso 1 1 calc R . .
C3B C 0.4803(5) 0.7446(4) 0.6530(3) 0.053(2) Uani 1 1 d . . .
H3B H 0.5005 0.8000 0.6545 0.064 Uiso 1 1 calc R . .
C4B C 0.4262(5) 0.7182(4) 0.6067(4) 0.055(2) Uani 1 1 d . . .
H4B H 0.4105 0.7564 0.5781 0.066 Uiso 1 1 calc R . .
C5B C 0.3956(4) 0.6348(4) 0.6032(3) 0.0413(17) Uani 1 1 d . . .
C6B C 0.4222(4) 0.5795(4) 0.6469(3) 0.0380(17) Uani 1 1 d . . .
C7B C 0.4149(4) 0.4341(4) 0.6130(3) 0.0366(16) Uani 1 1 d . . .
C8B C 0.3856(4) 0.3450(4) 0.6193(3) 0.0377(16) Uani 1 1 d . . .
C9B C 0.3961(4) 0.2691(4) 0.5943(3) 0.0410(17) Uani 1 1 d . . .
H9B H 0.4237 0.2682 0.5695 0.049 Uiso 1 1 calc R . .
C10B C 0.3640(4) 0.1939(4) 0.6076(3) 0.054(2) Uani 1 1 d . . .
H10B H 0.3707 0.1413 0.5920 0.065 Uiso 1 1 calc R . .
C11B C 0.3235(5) 0.1965(5) 0.6426(4) 0.078(3) Uani 1 1 d . . .
H11B H 0.3029 0.1456 0.6514 0.093 Uiso 1 1 calc R . .
C12B C 0.3118(5) 0.2758(5) 0.6664(4) 0.076(3) Uani 1 1 d . . .
C13B C 0.2699(7) 0.2939(5) 0.7050(5) 0.103(4) Uani 1 1 d . . .
C14B C 0.2419(11) 0.4023(6) 0.7606(8) 0.125(6) Uani 1 1 d . . .
C15B C 0.2842(10) 0.3936(8) 0.8156(8) 0.131(7) Uani 1 1 d . . .
C16B C 0.2524(11) 0.4170(8) 0.8569(7) 0.177(10) Uani 1 1 d . . .
H16B H 0.2775 0.4129 0.8931 0.212 Uiso 1 1 calc R . .
C17B C 0.1725(15) 0.4496(8) 0.8356(10) 0.187(12) Uani 1 1 d . . .
H17B H 0.1473 0.4652 0.8604 0.225 Uiso 1 1 calc R . .
C18B C 0.1361(15) 0.4573(9) 0.7844(11) 0.211(15) Uani 1 1 d . . .
H18B H 0.0888 0.4825 0.7743 0.253 Uiso 1 1 calc R . .
C19B C 0.1680(15) 0.4283(9) 0.7467(9) 0.152(9) Uani 1 1 d . . .
C20B C 0.5027(5) 0.5473(4) 0.7422(3) 0.0465(19) Uani 1 1 d . . .
H20B H 0.462(4) 0.507(5) 0.742(3) 0.056 Uiso 1 1 calc . . .
C21B C 0.5228(6) 0.5952(6) 0.7956(3) 0.077(3) Uani 1 1 d . . .
H21D H 0.5351 0.5538 0.8243 0.115 Uiso 1 1 calc R . .
H21E H 0.4808 0.6295 0.7982 0.115 Uiso 1 1 calc R . .
H21F H 0.5650 0.6324 0.7980 0.115 Uiso 1 1 calc R . .
C22B C 0.5685(5) 0.4939(5) 0.7373(3) 0.068(2) Uani 1 1 d . . .
H22D H 0.5565 0.4669 0.7028 0.102 Uiso 1 1 calc R . .
H22E H 0.5796 0.4499 0.7645 0.102 Uiso 1 1 calc R . .
H22F H 0.6113 0.5309 0.7416 0.102 Uiso 1 1 calc R . .
C23B C 0.3353(5) 0.6104(5) 0.5542(3) 0.055(2) Uani 1 1 d . . .
H23B H 0.318(4) 0.552(5) 0.559(3) 0.066 Uiso 1 1 calc . . .
C24B C 0.2670(6) 0.6720(6) 0.5452(4) 0.085(3) Uani 1 1 d . . .
H24D H 0.2826 0.7306 0.5416 0.128 Uiso 1 1 calc R . .
H24E H 0.2467 0.6683 0.5752 0.128 Uiso 1 1 calc R . .
H24F H 0.2295 0.6553 0.5133 0.128 Uiso 1 1 calc R . .
C25B C 0.3623(5) 0.6100(5) 0.5042(3) 0.071(3) Uani 1 1 d . . .
H25D H 0.3807 0.6666 0.4990 0.107 Uiso 1 1 calc R . .
H25E H 0.3215 0.5949 0.4738 0.107 Uiso 1 1 calc R . .
H25F H 0.4018 0.5681 0.5083 0.107 Uiso 1 1 calc R . .
C26B C 0.3642(10) 0.3602(14) 0.8332(7) 0.171(9) Uani 1 1 d . . .
H26B H 0.378(9) 0.344(10) 0.801(7) 0.205 Uiso 1 1 calc . . .
C27B C 0.3705(12) 0.2785(13) 0.8668(11) 0.259(14) Uani 1 1 d . . .
H27D H 0.4172 0.2790 0.8944 0.389 Uiso 1 1 calc R . .
H27E H 0.3686 0.2284 0.8445 0.389 Uiso 1 1 calc R . .
H27F H 0.3298 0.2764 0.8826 0.389 Uiso 1 1 calc R . .
C28B C 0.4196(12) 0.4288(14) 0.8617(7) 0.248(13) Uani 1 1 d . . .
H28D H 0.4037 0.4848 0.8465 0.371 Uiso 1 1 calc R . .
H28E H 0.4682 0.4159 0.8577 0.371 Uiso 1 1 calc R . .
H28F H 0.4220 0.4292 0.8990 0.371 Uiso 1 1 calc R . .
C29B C 0.133(2) 0.4426(15) 0.6998(18) 0.27(2) Uani 1 1 d . . .
H29B H 0.165(15) 0.418(14) 0.679(10) 0.327 Uiso 1 1 calc . . .
C30B C 0.1056(11) 0.5377(13) 0.6727(15) 0.36(2) Uani 1 1 d . . .
H30D H 0.1378 0.5823 0.6924 0.537 Uiso 1 1 calc R . .
H30E H 0.0551 0.5484 0.6735 0.537 Uiso 1 1 calc R . .
H30F H 0.1078 0.5379 0.6363 0.537 Uiso 1 1 calc R . .
C31B C 0.0455(14) 0.3896(13) 0.6759(8) 0.233(10) Uani 1 1 d . . .
H31D H 0.0490 0.3319 0.6904 0.349 Uiso 1 1 calc R . .
H31E H 0.0322 0.3865 0.6376 0.349 Uiso 1 1 calc R . .
H31F H 0.0080 0.4216 0.6867 0.349 Uiso 1 1 calc R . .
C32 C 0.000(3) 0.1505(18) 0.563(2) 0.56(5) Uani 1 1 d . . .
H32 H 0.02(3) 0.12(4) 0.60(2) 0.674 Uiso 1 1 calc . . .
C33 C 0.1944(13) 0.4053(15) 0.5345(10) 0.214(8) Uiso 1 1 d U . .
C34 C 0.2383(17) 0.368(2) 0.4881(13) 0.260(12) Uiso 1 1 d U . .
C35 C 0.1920(18) 0.335(2) 0.4525(13) 0.276(13) Uiso 1 1 d U . .
C36 C 0.176(2) 0.458(2) 0.4246(16) 0.359(19) Uiso 1 1 d U . .
Cl1 Cl 0.0000(5) 0.0802(6) 0.5174(4) 0.305(4) Uani 1 1 d . . .
Cl2 Cl -0.0775(5) 0.2008(8) 0.5589(4) 0.370(6) Uani 1 1 d . . .
Cl3 Cl 0.0643(11) 0.2295(9) 0.5539(12) 0.682(18) Uani 1 1 d . . .
N1A N 0.2567(3) 0.2652(3) 0.2962(2) 0.0378(14) Uani 1 1 d . . .
N2A N 0.3437(3) 0.2831(3) 0.3865(2) 0.0335(13) Uani 1 1 d . . .
N3A N 0.3406(3) 0.1350(3) 0.4208(2) 0.0320(13) Uani 1 1 d . . .
N1B N 0.3931(3) 0.4920(3) 0.6449(2) 0.0380(13) Uani 1 1 d . . .
N2B N 0.3460(4) 0.3459(3) 0.6549(3) 0.0552(18) Uani 1 1 d . . .
N3B N 0.2772(5) 0.3759(4) 0.7208(4) 0.097(3) Uani 1 1 d . . .
Ni1A Ni 0.29187(5) 0.18854(5) 0.35485(3) 0.0334(3) Uani 1 1 d . . .
Ni1B Ni 0.33249(6) 0.44726(5) 0.68583(4) 0.0559(4) Uani 1 1 d . . .
O4 O 0.2397(3) 0.9296(3) 0.3285(2) 0.0603(15) Uani 1 1 d . . .
O5 O 0.1639(7) 0.0905(7) 0.6752(5) 0.184(5) Uani 1 1 d . . .
O6 O 0.3176(4) 0.7120(3) 0.6927(3) 0.097(2) Uani 1 1 d . . .
O7 O 0.127(3) 0.449(3) 0.483(2) 0.68(3) Uiso 1 1 d U . .
O1A O 0.2657(3) 0.4091(3) 0.27240(19) 0.0564(14) Uani 1 1 d . . .
O2A O 0.4252(3) 0.1666(3) 0.50323(18) 0.0400(11) Uani 1 1 d . . .
O3A O 0.2334(3) 0.0939(3) 0.32095(18) 0.0477(13) Uani 1 1 d . . .
O1B O 0.2377(5) 0.2333(4) 0.7226(4) 0.135(4) Uani 1 1 d . . .
O2B O 0.4565(3) 0.4461(3) 0.58382(18) 0.0400(11) Uani 1 1 d . . .
O3B O 0.3157(3) 0.5513(3) 0.7182(2) 0.0612(16) Uani 1 1 d . . .
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
C1A C6A 1.390(10) . ?
C1A C2A 1.399(10) . ?
C1A C20A 1.497(11) . ?
C2A C3A 1.361(11) . ?
C3A C4A 1.389(11) . ?
C4A C5A 1.391(10) . ?
C5A C6A 1.402(9) . ?
C5A C23A 1.509(10) . ?
C6A N1A 1.454(8) . ?
C7A O1A 1.245(7) . ?
C7A N1A 1.338(8) . ?
C7A C8A 1.501(10) . ?
C8A N2A 1.342(7) . ?
C8A C9A 1.375(9) . ?
C9A C10A 1.357(10) . ?
C10A C11A 1.384(9) . ?
C11A C12A 1.375(8) . ?
C12A N2A 1.329(8) . ?
C12A C13A 1.511(8) . ?
C13A O2A 1.240(7) . ?
C13A N3A 1.352(8) . ?
C14A C19A 1.395(9) . ?
C14A C15A 1.406(9) . ?
C14A N3A 1.436(7) . ?
C15A C16A 1.417(10) . ?
C15A C26A 1.503(12) . ?
C16A C17A 1.344(11) . ?
C17A C18A 1.368(11) . ?
C18A C19A 1.414(9) . ?
C19A C29A 1.495(10) . ?
C20A C22A 1.480(12) . ?
C20A C21A 1.488(12) . ?
C23A C25A 1.510(11) . ?
C23A C24A 1.515(10) . ?
C26A C28A 1.521(12) . ?
C26A C27A 1.526(15) . ?
C29A C31A 1.493(10) . ?
C29A C30A 1.522(10) . ?
C1B C2B 1.398(9) . ?
C1B C6B 1.406(10) . ?
C1B C20B 1.528(10) . ?
C2B C3B 1.351(10) . ?
C3B C4B 1.397(11) . ?
C4B C5B 1.398(9) . ?
C5B C6B 1.397(9) . ?
C5B C23B 1.493(11) . ?
C6B N1B 1.448(8) . ?
C7B O2B 1.242(8) . ?
C7B N1B 1.357(8) . ?
C7B C8B 1.501(9) . ?
C8B N2B 1.338(8) . ?
C8B C9B 1.377(9) . ?
C9B C10B 1.392(9) . ?
C10B C11B 1.336(11) . ?
C11B C12B 1.413(10) . ?
C12B N2B 1.329(9) . ?
C12B C13B 1.462(11) . ?
C13B O1B 1.263(9) . ?
C13B N3B 1.323(10) . ?
C14B C19B 1.38(3) . ?
C14B N3B 1.434(12) . ?
C14B C15B 1.44(2) . ?
C15B C16B 1.412(15) . ?
C15B C26B 1.52(3) . ?
C16B C17B 1.52(3) . ?
C17B C18B 1.32(4) . ?
C18B C19B 1.36(2) . ?
C19B C29B 1.23(5) . ?
C20B C22B 1.509(11) . ?
C20B C21B 1.527(11) . ?
C23B C25B 1.524(11) . ?
C23B C24B 1.549(11) . ?
C26B C27B 1.52(3) . ?
C26B C28B 1.519(18) . ?
C29B C30B 1.64(3) . ?
C29B C31B 1.77(4) . ?
C32 Cl1 1.61(4) . ?
C32 Cl2 1.62(4) . ?
C32 Cl3 1.77(4) . ?
C33 O7 1.69(6) . ?
C33 C34 1.74(3) . ?
C34 C35 1.18(3) . ?
C35 C36 2.02(4) . ?
C36 O7 1.98(5) . ?
N1A Ni1A 1.896(5) . ?
N2A Ni1A 1.813(5) . ?
N3A Ni1A 1.893(5) . ?
N1B Ni1B 1.886(5) . ?
N2B Ni1B 1.807(5) . ?
N3B Ni1B 1.903(6) . ?
Ni1A O3A 1.884(4) . ?
Ni1B O3B 1.876(4) . ?
