#------------------------------------------------------------------------------
#$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $
#$Revision: 853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2200052.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_2200052
_journal_name_full  'Acta Crystallographica, Section E'
_journal_year  2001
_journal_volume  57
_journal_page_first  m48
_journal_page_last  m50
_publ_section_title
;
[(1RS,4RS)-5,5,7,13,15,15-Hexamethyl-1,4,8,12-tetraazacyclopentadeca-
7,12-diene-N^1^,N^4^,N^8^,N^12^]nickel(II) diperchlorate
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
loop_
_publ_author_name
  'Curtis, Neil F.'
  'Waters, Joyce M.'
  'Rickard, Clifton E.'
_chemical_formula_moiety  'C17 H34 N4 Ni1 2+, 2Cl1 O4 1-'
_chemical_formula_sum  'C17 H34 Cl2 N4 Ni O8'
_chemical_formula_iupac  '[Ni (C17 H34 N4)](Cl1 O4)2'
_chemical_formula_weight  552.09
_symmetry_cell_setting  monoclinic
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'
_cell_length_a  10.35290(10)
_cell_length_b  16.11280(10)
_cell_length_c  15.04000(10)
_cell_angle_alpha  90.00
_cell_angle_beta  107.0250(10)
_cell_angle_gamma  90.00
_cell_volume  2398.94(3)
_cell_formula_units_Z  4
_cell_measurement_temperature  203(2)
_exptl_crystal_density_diffrn  1.529
_diffrn_ambient_temperature  203(2)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
  Ni  .48685(3)  .07048(2)  .22713(2)  .02468(10) Uani d . 1 . Ni
  N1  .3671(2)  -.00883(13)  .25706(15)  .0295(4) Uani d . 1 . N
  H1  .3292(2)  .01636(13)  .29833(15)  .050 Uiso calc R 1 1 H
  C2  .4522(3)  -.0785(2)  .3073(2)  .0436(7) Uani d . 1 . C
  H2A  .4780(3)  -.1150(2)  .2632(2)  .080 Uiso calc R 1 . H
  H2B  .4025(3)  -.1113(2)  .3413(2)  .080 Uiso calc R 1 . H
  C3  .5754(3)  -.0405(2)  .3736(2)  .0441(7) Uani d . 1 . C
  H3A  .5510(3)  -.0111(2)  .4234(2)  .080 Uiso calc R 1 . H
  H3B  .6414(3)  -.0837(2)  .4016(2)  .080 Uiso calc R 1 . H
  N4  .6333(2)  .01842(13)  .3191(2)  .0310(5) Uani d . 1 . N
  H4  .6817(2)  -.01217(13)  .2882(2)  .050 Uiso calc R 1 1 H
  C5  .7283(3)  .0822(2)  .3781(2)  .0352(6) Uani d . 1 . C
  C51  .6467(3)  .1436(2)  .4166(2)  .0428(7) Uani d . 1 . C
  H51A  .6005(3)  .1143(2)  .4547(2)  .080 Uiso calc R 1 . H
  H51B  .5807(3)  .1708(2)  .3656(2)  .080 Uiso calc R 1 . H
  H51C  .7068(3)  .1848(2)  .4541(2)  .080 Uiso calc R 1 . H
  C52  .8342(3)  .0388(2)  .4572(2)  .0556(9) Uani d . 1 . C
  H52A  .8852(3)  .0000(2)  .4314(2)  .080 Uiso calc R 1 . H
  H52B  .7896(3)  .0091(2)  .4960(2)  .080 Uiso calc R 1 . H
  H52C  .8951(3)  .0799(2)  .4944(2)  .080 Uiso calc R 1 . H
  C6  .8035(3)  .1250(2)  .3173(2)  .0409(7) Uani d . 1 . C
  H6A  .8596(3)  .1685(2)  .3552(2)  .050 Uiso calc R 1 . H
  H6B  .8652(3)  .0840(2)  .3040(2)  .050 Uiso calc R 1 . H
  C7  .7276(3)  .1634(2)  .2272(2)  .0491(8) Uani d . 1 . C
  C71  .8180(3)  .2065(3)  .1789(3)  .0630(10) Uani d . 1 . C
  H71A  .7633(3)  .2303(3)  .1208(3)  .080 Uiso calc R 1 . H
  H71B  .8807(3)  .1667(3)  .1664(3)  .080 Uiso calc R 1 . H
  H71C  .8681(3)  .2503(3)  .2186(3)  .080 Uiso calc R 1 . H
  N8  .6126(2)  .1267(2)  .1768(2)  .0398(6) Uani d . 1 . N
  C9  .5470(3)  .1537(2)  .0801(2)  .0395(6) Uani d . 1 . C
  H9A  .4927(3)  .1080(2)  .0453(2)  .080 Uiso calc R 1 . H
  H9B  .6165(3)  .1675(2)  .0501(2)  .080 Uiso calc R 1 . H
  C10  .4574(4)  .2285(2)  .0773(2)  .0491(8) Uani d . 1 . C
  H10A  .5123(4)  .2789(2)  .0847(2)  .080 Uiso calc R 1 . H
  H10B  .3894(4)  .2310(2)  .0163(2)  .080 Uiso calc R 1 . H
  C11  .3868(3)  .2262(2)  .1522(2)  .0377(6) Uani d . 1 . C
  H11A  .4494(3)  .2452(2)  .2110(2)  .080 Uiso calc R 1 . H
  H11B  .3098(3)  .2644(2)  .1356(2)  .080 Uiso calc R 1 . H
  N12  .3382(2)  .1419(2)  .1652(2)  .0405(6) Uani d . 1 . N
  C13  .2147(3)  .1171(2)  .1159(2)  .0459(8) Uani d . 1 . C
  C131  .1055(3)  .1801(2)  .0762(2)  .0498(8) Uani d . 1 . C
  H13A  .1455(3)  .2303(2)  .0602(2)  .080 Uiso calc R 1 . H
  H13B  .0592(3)  .1931(2)  .1220(2)  .080 Uiso calc R 1 . H
  H13C  .0414(3)  .1576(2)  .0209(2)  .080 Uiso calc R 1 . H
  C14  .1597(3)  .0386(2)  .1419(2)  .0376(6) Uani d . 1 . C
  H14A  .0859(3)  .0208(2)  .0880(2)  .050 Uiso calc R 1 . H
  H14B  .1193(3)  .0519(2)  .1915(2)  .050 Uiso calc R 1 . H
  C15  .2523(3)  -.0362(2)  .1743(2)  .0339(6) Uani d . 1 . C
  C151  .1699(3)  -.1040(2)  .2044(3)  .0477(8) Uani d . 1 . C
  H15A  .1354(3)  -.0828(2)  .2534(3)  .080 Uiso calc R 1 . H
  H15B  .2272(3)  -.1517(2)  .2273(3)  .080 Uiso calc R 1 . H
  H15C  .0949(3)  -.1205(2)  .1517(3)  .080 Uiso calc R 1 . H
  C152  .3075(3)  -.0680(2)  .0975(2)  .0421(7) Uani d . 1 . C
  H15D  .3658(3)  -.1153(2)  .1200(2)  .080 Uiso calc R 1 . H
  H15E  .3588(3)  -.0244(2)  .0790(2)  .080 Uiso calc R 1 . H
  H15F  .2331(3)  -.0846(2)  .0444(2)  .080 Uiso calc R 1 . H
  Cl1  .77772(9)  -.09388(7)  .15944(7)  .0601(2) Uani d PD  .877(7) 1 Cl
  O11  .8237(4)  -.1649(3)  .1282(4)  .101(2) Uani d PD  .877(7) 1 O
  O12  .6406(5)  -.0874(6)  .1386(6)  .189(5) Uani d PD  .877(7) 1 O
  O13  .8290(6)  -.0227(3)  .1248(4)  .135(2) Uani d PD  .877(7) 1 O
  O14  .8332(4)  -.0909(3)  .2582(3)  .094(2) Uani d PD  .877(7) 1 O
  Cl11  .77772(9)  -.09388(7)  .15944(7)  .0601(2) Uani d PD  .123(7) 2 Cl
  O15  .821(2)  -.1052(17)  .0771(15)  .073(8) Uiso d PD  .123(7) 2 O
  O16  .849(2)  -.0370(14)  .2240(15)  .056(6) Uiso d PD  .123(7) 2 O
  O17  .778(5)  -.176(2)  .203(3)  .35(6)  Uiso d PD  .123(7) 2 O
  O18  .631(3)  -.0703(15)  .1312(19)  .046(6) Uiso d PD  .123(7) 2 O
  Cl2  .23467(8)  .16963(5)  .40219(5)  .0432(2) Uani d PD  .855(8) 1 Cl
  O21  .3456(4)  .2205(3)  .4528(3)  .0865(15) Uani d PD  .855(8) 1 O
  O22  .1775(5)  .2026(3)  .3119(2)  .0719(11) Uani d PD  .855(8) 1 O
  O23  .2872(5)  .0877(2)  .3974(2)  .0690(13) Uani d PD  .855(8) 1 O
  O24  .1387(4)  .1676(3)  .4535(3)  .0645(10) Uani d PD  .855(8) 1 O
  Cl21  .23467(8)  .16963(5)  .40219(5)  .0432(2) Uani d PD  .145(8) 2 Cl
  O25  .186(2)  .0849(11)  .3588(14)  .068(6) Uiso d PD  .145(8) 2 O
  O26  .359(2)  .1822(19)  .400(2)  .118(11) Uiso d PD  .145(8) 2 O
  O27  .189(2)  .1782(13)  .4747(13)  .048(6) Uiso d PD  .145(8) 2 O
  O28  .143(2)  .2234(14)  .3266(15)  .058(6) Uiso d PD  .145(8) 2 O
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
  Ni  .0216(2)  .0245(2)  .0277(2)  .00088(11)  .00687(12)  .00188(12)
  N1  .0321(11)  .0277(11)  .0294(11)  -.0039(9)  .0103(9)  -.0021(8)
  C2  .048(2)  .0306(14)  .047(2)  -.0058(12)  .0049(13)  .0084(12)
  C3  .049(2)  .0362(15)  .039(2)  -.0045(13)  .0007(13)  .0122(12)
  N4  .0311(11)  .0269(11)  .0320(11)  .0026(9)  .0047(9)  -.0015(9)
  C5  .0285(13)  .0380(15)  .0341(14)  -.0001(11)  .0013(11)  -.0015(11)
  C51  .046(2)  .041(2)  .040(2)  -.0070(13)  .0123(13)  -.0118(13)
  C52  .044(2)  .058(2)  .050(2)  -.001(2)  -.0107(15)  .009(2)
  C6  .0238(12)  .049(2)  .048(2)  -.0034(12)  .0068(12)  -.0026(13)
  C7  .0291(14)  .068(2)  .050(2)  -.0083(14)  .0111(13)  .014(2)
  C71  .039(2)  .086(3)  .069(2)  -.017(2)  .023(2)  .013(2)
  N8  .0291(11)  .0460(14)  .0414(13)  -.0053(10)  .0057(10)  .0123(11)
  C9  .0396(15)  .048(2)  .0325(14)  .0025(13)  .0128(12)  .0060(12)
  C10  .057(2)  .044(2)  .052(2)  .0111(15)  .025(2)  .0204(14)
  C11  .0368(14)  .0295(14)  .048(2)  .0046(11)  .0139(12)  .0088(12)
  N12  .0278(11)  .0349(13)  .054(2)  .0014(10)  .0045(10)  .0141(11)
  C13  .0248(13)  .051(2)  .061(2)  .0048(12)  .0108(13)  .0187(15)
  C131  .0300(14)  .063(2)  .057(2)  .0129(14)  .0142(13)  .023(2)
  C14  .0243(12)  .048(2)  .041(2)  -.0033(11)  .0104(11)  -.0026(12)
  C15  .0287(13)  .0368(14)  .0367(14)  -.0071(11)  .0103(11)  -.0063(11)
  C151  .040(2)  .043(2)  .064(2)  -.0130(13)  .0211(15)  -.0061(15)
  C152  .040(2)  .047(2)  .040(2)  -.0045(13)  .0131(12)  -.0139(13)
  Cl1  .0452(4)  .0704(6)  .0663(6)  .0102(4)  .0185(4)  -.0217(5)
  O11  .095(3)  .071(3)  .150(4)  .005(2)  .055(3)  -.055(3)
  O12  .041(2)  .354(12)  .158(6)  .031(4)  .007(3)  -.147(7)
  O13  .143(5)  .091(4)  .172(6)  .012(3)  .046(4)  .055(3)
  O14  .094(3)  .114(4)  .067(2)  .029(3)  .014(2)  -.007(2)
  Cl11  .0452(4)  .0704(6)  .0663(6)  .0102(4)  .0185(4)  -.0217(5)
  Cl2  .0469(4)  .0430(4)  .0454(4)  .0013(3)  .0226(3)  .0007(3)
  O21  .055(2)  .090(3)  .102(3)  -.024(2)  .003(2)  -.018(2)
  O22  .103(3)  .072(2)  .040(2)  .015(2)  .021(2)  .005(2)
  O23  .105(3)  .057(2)  .056(2)  .028(2)  .041(2)  -.0021(14)
  O24  .049(2)  .089(3)  .065(2)  .001(2)  .033(2)  -.008(2)
  Cl21  .0469(4)  .0430(4)  .0454(4)  .0013(3)  .0226(3)  .0007(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
  Ni N8 . 1.915(2) yes
  Ni N4 . 1.920(2) yes
  Ni N1 . 1.924(2) yes
  Ni N12 . 1.929(2) yes
  N1 C2 . 1.489(4) ?
  N1 C15 . 1.513(3) ?
  N1 O23 . 2.929(3) ?
  N1 O25 . 3.13(2) ?
  N1 H1 .  .92 ?
  C2 C3 . 1.499(4) ?
  C2 H2A .  .98 ?
  C2 H2B .  .98 ?
  C3 N4 . 1.491(4) ?
  C3 H3A .  .98 ?
  C3 H3B .  .98 ?
  N4 C5 . 1.516(3) ?
  N4 O14 . 3.054(5) ?
  N4 O16 . 3.11(2) ?
  N4 H4 .  .92 ?
  C5 C51 . 1.521(4) ?
  C5 C6 . 1.528(4) ?
  C5 C52 . 1.531(4) ?
  C51 H51A .  .97 ?
  C51 H51B .  .97 ?
  C51 H51C .  .97 ?
  C52 H52A .  .97 ?
  C52 H52B .  .97 ?
  C52 H52C .  .97 ?
  C6 C7 . 1.489(4) ?
  C6 H6A .  .98 ?
  C6 H6B .  .98 ?
  C7 N8 . 1.346(4) yes
  C7 C71 . 1.511(4) ?
  C71 H71A .  .97 ?
  C71 H71B .  .97 ?
  C71 H71C .  .97 ?
  N8 C9 . 1.478(4) ?
  C9 C10 . 1.514(4) ?
  C9 H9A .  .98 ?
  C9 H9B .  .98 ?
  C10 C11 . 1.513(4) ?
  C10 H10A .  .98 ?
  C10 H10B .  .98 ?
  C11 N12 . 1.480(4) ?
  C11 H11A .  .98 ?
  C11 H11B .  .98 ?
  N12 C13 . 1.338(4) yes
  C13 C14 . 1.487(4) ?
  C13 C131 . 1.507(4) ?
  C131 H13A .  .97 ?
  C131 H13B .  .97 ?
  C131 H13C .  .97 ?
  C14 C15 . 1.528(4) ?
  C14 H14A .  .98 ?
  C14 H14B .  .98 ?
  C15 C152 . 1.521(4) ?
  C15 C151 . 1.535(4) ?
  C151 H15A .  .97 ?
  C151 H15B .  .97 ?
  C151 H15C .  .97 ?
  C152 H15D .  .97 ?
  C152 H15E .  .97 ?
  C152 H15F .  .97 ?
  Cl1 O12 . 1.365(5) ?
  Cl1 O11 . 1.375(3) ?
  Cl1 O13 . 1.425(5) ?
  Cl1 O14 . 1.428(4) ?
  Cl11 O16 . 1.38(2) ?
  Cl11 O15 . 1.44(2) ?
  Cl11 O17 . 1.47(3) ?
  Cl11 O18 . 1.50(2) ?
  Cl2 O22 . 1.416(3) ?
  Cl2 O24 . 1.426(3) ?
  Cl2 O21 . 1.434(3) ?
  Cl2 O23 . 1.438(3) ?
  Cl21 O26 . 1.31(2) ?
  Cl21 O27 . 1.32(2) ?
  Cl21 O28 . 1.52(2) ?
  Cl21 O25 . 1.53(2) ?