#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/95/2009584.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009584
loop_
_publ_author_name
'Tahirov, T.H.'
'Lu, T.-H.'
'Shu, K.'
'Chung, C.-S.'
_publ_section_title
;[(4RS,7SR,11RS)-4,12-Dimethyl-4,7,11-triazatridecylamine-N,N',N'',N''']nickel(II)
 diperchlorate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              516
_journal_page_last               518
_journal_paper_doi               10.1107/S0108270193009795
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C12 H30 Cl2 N4 Ni O8'
_chemical_formula_weight         488.0
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.491(4)
_cell_length_b                   14.679(4)
_cell_length_c                   16.827(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(3)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      6.07
_cell_volume                     2097.3(12)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3430
_diffrn_reflns_theta_max         29.9
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.23
_exptl_absorpt_correction_T_max  0.87217
_exptl_absorpt_correction_T_min  0.87147
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       parallelepiped
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.35
_refine_ls_goodness_of_fit_obs   0.59
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     261
_refine_ls_number_reflns         1924
_refine_ls_R_factor_obs          0.055
_refine_ls_shift/esd_max         0.78
_refine_ls_structure_factor_coef 'F; structure-factor coefficient 2.978(7)'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.054
_reflns_number_observed          1924
_reflns_number_total             3430
_reflns_observed_criterion       I>=2.5\s(I)
_cod_data_source_file            as1060.cif
_cod_data_source_block           as1060_structure_1_of_1
_cod_original_cell_volume        2097.0(10)
_cod_original_formula_sum        'C12 H30 Cl2 N4 Ni1 O8'
_cod_database_code               2009584
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Ni .24397(14) .80566(7) .22878(5) 1.0
Cl(1) .7905(3) .65783(19) .18758(17) 1.0
Cl(2) .7010(4) .0539(2) .07441(17) 1.0
O(1) .7069(12) .7291(6) .2195(10) 1.0
O(2) .6908(13) .5845(6) .1929(10) 1.0
O(3) .817(2) .6730(17) .1146(7) 1.0
O(4) .9302(11) .6422(7) .2275(7) 1.0
O(5) .743(2) -.0367(7) .0833(9) 0.85
O(5') .692(6) .007(3) .149(3) 0.15
O(6) .713(4) .0727(16) -.0015(9) 0.70
O(6') .596(4) .028(3) .0201(19) 0.30
O(7) .567(3) .095(2) .0970(17) 0.70
O(7') .600(6) .044(3) .137(3) 0.30
O(8) .8190(14) .1081(8) .1101(9) 1.0
N(1) .2128(9) .8053(5) .3437(4) 1.0
N(2) .1431(9) .9221(5) .2227(5) 1.0
N(3) .2691(9) .8115(6) .1137(4) 1.0
N(4) .3555(9) .6915(5) .2345(4) 1.0
C(1) .3018(19) .8563(10) .4795(6) 1.0
C(2) .31396(14) .8673(8) .3909(6) 1.0
C(3) .4803(18) .8570(12) .3627(9) 1.0
C(4) .0387(12) .8128(8) .3627(6) 1.0
C(5) -.0364(12) .8984(8) .3370(7) 1.0
C(6) -.0256(12) .9166(7) .2476(6) 1.0
C(7) .1594(14) .9618(7) .1409(6) 1.0
C(8) .1531(15) .8790(9) .0846(6) 1.0
C(9) .4282(15) .8428(10) .0963(7) 1.0
C(10) .2395(18) .7258(8) .0700(6) 1.0
C(11) .3341(15) .6454(8) .0947(7) 1.0
C(12) .3070(13) .6176(7) .1765(8) 1.0
H(N1) .219 .736 .361 1.0
H(N2) .207 .965 .265 1.0
H(N41) .342 .664 .294 1.0
H(N42) .481 .705 .225 1.0
H(1) .261 .905 .511 1.0
H(2) .217 .808 .492 1.0
H(3) .426 .831 .499 1.0
H(4) .278 .938 .375 1.0
H(5) .567 .862 .410 1.0
H(6) .512 .903 .316 1.0
H(7) .483 .792 .342 1.0
H(8) .020 .805 .426 1.0
H(9) -.024 .757 .332 1.0
H(10) -.160 .896 .355 1.0
H(11) .021 .953 .369 1.0
H(12) -.086 .981 .235 1.0
H(13) -.086 .863 .216 1.0
H(14) .069 1.011 .127 1.0
H(15) .274 .997 .133 1.0
H(16) .175 .898 .025 1.0
H(17) .034 .850 .089 1.0
H(18) .451 .911 .119 1.0
H(19) .456 .842 .034 1.0
H(20) .504 .798 .125 1.0
H(21) .255 .737 .006 1.0
H(22) .115 .706 .079 1.0
H(23) .315 .590 .055 1.0
H(24) .459 .668 .088 1.0
H(25) .186 .603 .185 1.0
H(26) .378 .557 .189 1.0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) Ni N(2) 89.7(3) yes
N(1) Ni N(3) 177.2(3) yes
N(1) Ni N(4) 90.8(3) yes
N(2) Ni N(3) 87.5(3) yes
N(2) Ni N(4) 177.1(3) yes
N(3) Ni N(4) 92.0(3) yes
O(1) Cl(1) O(2) 104.7(7) no
O(1) Cl(1) O(3) 110.0(10) no
O(1) Cl(1) O(4) 112.3(8) no
O(2) Cl(1) O(3) 108.0(10) no
O(2) Cl(1) O(4) 111.6(7) no
O(3) Cl(1) O(4) 111.0(10) no
O(5) Cl(2) O(6) 107.0(10) no
O(5) Cl(2) O(7) 128(2) no
O(5) Cl(2) O(8) 108.2(9) no
O(6) Cl(2) O(7) 104(2) no
O(6) Cl(2) O(8) 104(2) no
Ni N(1) C(2) 116.8(6) yes
Ni N(1) C(4) 109.9(5) yes
C(2) N(1) C(4) 114.0(8) yes
Ni N(2) C(6) 111.4(6) yes
Ni N(2) C(7) 110.7(6) yes
C(6) N(2) C(7) 111.5(7) yes
Ni N(3) C(8) 106.6(6) yes
Ni N(3) C(9) 108.3(6) yes
N N(3) C(10) 115.9(6) yes
C(8) N(3) C(9) 109.9(9) yes
C(8) N(3) C(10) 107.0(8) yes
C(9) N(3) C(10) 109.0(9) yes
Ni N(4) C(12) 117.1(6) yes
N(1) C(2) C(1) 115.0(10) yes
N(1) C(2) C(3) 108.3(9) yes
C(1) C(2) C(3) 112.0(10) yes
N(1) C(4) C(5) 114.9(8) yes
C(4) C(5) C(6) 114.3(9) yes
N(2) C(6) C(5) 110.0(8) yes
N(2) C(7) C(8) 104.8(8) yes
N(3) C(8) C(7) 107.5(8) yes
N(3) C(10) C(11) 116.4(9) yes
C(10) C(11) C(12) 113.7(9) yes
N(4) C(12) C(11) 111.4(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N(1) 1.951(6) yes
Ni N(2) 1.915(7) yes
Ni N(3) 1.951(6) yes
Ni N(4) 1.927(8) yes
Cl(1) O(1) 1.370(10) no
Cl(1) O(2) 1.370(10) no
Cl(1) O(3) 1.270(10) no
Cl(1) O(4) 1.382(9) no
Cl(2) O(5) 1.390(10) no
Cl(2) O(6) 1.31(6) no
Cl(2) O(7) 1.34(2) no
Cl(2) O(8) 1.410(10) no
N(1) C(2) 1.480(10) yes
N(1) C(4) 1.520(10) yes
N(2) C(6) 1.490(10) yes
N(2) C(7) 1.500(10) yes
N(3) C(8) 1.48(2) yes
N(3) C(9) 1.46(2) yes
N(3) C(10) 1.480(10) yes
N(4) C(12) 1.520(10) yes
C(1) C(2) 1.50(2) yes
C(2) C(3) 1.50(2) yes
C(4) C(5) 1.47(2) yes
C(5) C(6) 1.53(2) yes
C(7) C(8) 1.54(2) yes
C(10) C(11) 1.49(2) yes
C(11) C(12) 1.45(2) yes
