#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/59/2005936.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_2005936
loop_
_publ_author_name
'Lu, T.-H.'
'Tahirov, T. H.'
'Shu, K.'
'Chung, C.-S.'
_publ_section_title
;
 Copper(II) and Nickel(II) Complexes of
 4-Methyl-4,7-diazadecane-1,10-diamine
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              204
_journal_page_last               206
_journal_paper_doi               10.1107/S0108270196006129
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C9 H24 Cl2 N4 Ni O8'
_chemical_formula_weight         445.92
_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'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 100.14(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.732(1)
_cell_length_b                   14.800(2)
_cell_length_c                   13.655(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(3)
_cell_measurement_theta_max      17.17
_cell_measurement_theta_min      7.52
_cell_volume                     1737.1(5)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5252
_diffrn_reflns_theta_max         29.9
_diffrn_standards_decay_%        +-0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.47
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   'empirical (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.10(8)
_refine_diff_density_min         -1.72(8)
_refine_ls_extinction_coef       '0.09(1) (length in mm)'
_refine_ls_extinction_method     'Zachariasen (1968)'
_refine_ls_goodness_of_fit_obs   1.24
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4056
_refine_ls_R_factor_obs          0.078
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.087
_reflns_number_observed          4056
_reflns_number_total             5066
_reflns_observed_criterion       I>=1.5\s(I)
_cod_data_source_file            hr1023.cif
_cod_data_source_block           hr1023b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005936
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
Ni .20043(8) .73874(5) .09114(5) 2.38(3)
Cl(1) -.14018(19) .72628(13) -.12171(12) 3.79(7)
Cl(2) -.10772(2) .98899(13) .19949(15) 4.23(7)
O(1) -.0248(8) .6669(5) -.0703(5) 7.4(4)
O(2) -.1033(10) .7494(7) -.2144(5) 9.1(5)
O(3) -.2853(8) .6826(6) -.1404(6) 8.4(4)
O(4) -.1519(9) .8037(5) -.0642(6) 7.8(4)
O(5) -.1700(11) 1.0753(5) .1811(7) 9.2(5)
O(6) .0544(8) .9879(6) .2156(6) 8.4(4)
O(7) -.1569(13) .9581(8) .2829(10) 16.5(10)
O(8) -.1510(14) .9375(9) .1149(10) 16.2(8)
N(1) .0219(5) .7529(4) .1563(4) 3.2(2)
N(2) .2308(6) .6127(4) .1295(4) 3.3(2)
N(3) .3826(6) .7257(4) .0270(4) 3.3(2)
N(4) .1808(7) .8649(4) .0554(5) 3.7(2)
C(1) -.0797(9) .6786(6) .1760(6) 4.6(4)
C(2) .0077(10) .5961(7) .2176(6) 5.4(4)
C(3) .1036(10) .5541(5) .1467(6) 4.5(3)
C(4) .3251(10) .5706(5) .0614(6) 4.2(3)
C(5) .4499(10) .6348(6) .0530(7) 4.7(3)
C(6) .3360(9) .7285(6) -.0818(5) 4.5(3)
C(7) .5066(8) .7948(6) .0618(6) 4.4(3)
C(8) .4520(10) .8911(6) .0369(7) 5.0(4)
C(9) .3215(10) .9408(5) .0853(6) 4.6(3)
H(N11) -.049 .794 .107 4.7
H(N12) .067 .782 .215 4.7
H(N2) .313 .622 .193 4.7
H(N41) .094 .892 .089 4.7
H(N42) .160 .869 -.020 4.7
H(1) -.142 .703 .234 4.7
H(2) .352 .658 .115 4.7
H(3) -.079 .545 .229 4.7
H(4) .096 .610 .286 4.7
H(5) .140 .493 .169 4.7
H(6) .023 .553 .075 4.7
H(7) .250 .568 .003 4.7
H(8) .371 .513 .073 4.7
H(9) .517 .636 .124 4.7
H(10) .525 .611 .008 4.7
H(11) .432 .727 -.115 4.7
H(12) .270 .790 -.098 4.7
H(13) .261 .666 -.116 4.7
H(14) .599 .775 .035 4.7
H(15) .551 .772 .141 4.7
H(16) .416 .897 -.044 4.7
H(17) .550 .937 .058 4.7
H(18) .316 .982 .069 4.7
H(19) .351 .907 .156 4.7
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle
_geom_angle_publ_flag
O(1) Ni O(2) 2_454 . 159.2(3) yes
O(1) Ni N(1) 2_454 . 84.0(2) yes
O(1) Ni N(2) 2_454 . 84.0(2) yes
O(1) Ni N(3) 2_454 . 96.9(2) yes
O(1) Ni N(4) 2_454 . 98.4(2) yes
O(2) Ni N(1) . . 88.1(2) yes
O(2) Ni N(2) . . 77.3(3) yes
O(2) Ni N(3) . . 91.1(2) yes
O(2) Ni N(4) . . 100.6(3) yes
N(1) Ni N(2) . . 93.6(2) yes
N(1) Ni N(3) . . 179.1(2) yes
N(1) Ni N(4) . . 88.2(2) yes
N(2) Ni N(3) . . 86.7(2) yes
N(2) Ni N(4) . . 177.2(2) yes
N(3) Ni N(4) . . 91.5(2) yes
Ni O(1) Cl(1) . 2_454 118.4(4) yes
Ni O(2) Cl(1) . . 130.4(5) yes
Ni N(1) C(1) . . 124.3(5) yes
Ni N(2) C(3) . . 122.8(5) yes
Ni N(2) C(4) . . 107.3(4) yes
C(3) N(2) C(4) . . 111.9(6) yes
Ni N(3) C(5) . . 107.5(4) yes
Ni N(3) C(6) . . 110.3(4) yes
Ni N(3) C(7) . . 112.9(4) yes
C(5) N(3) C(6) . . 107.1(6) yes
C(5) N(3) C(7) . . 108.0(6) yes
C(6) N(3) C(7) . . 110.8(6) yes
Ni N(4) C(9) . . 116.1(5) yes
N(1) C(1) C(2) . . 113.4(6) yes
C(1) C(2) C(3) . . 113.2(6) yes
N(2) C(3) C(2) . . 112.3(7) yes
N(2) C(4) C(5) . . 106.2(6) yes
N(3) C(5) C(4) . . 109.7(6) yes
N(3) C(7) C(8) . . 112.7(6) yes
C(7) C(8) C(9) . . 114.4(7) yes
N(4) C(9) C(8) . . 112.2(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni . O(1) 2_454 2.886(7) yes
Ni . O(2) . 2.901(7) yes
Ni . N(1) . 1.938(5) yes
Ni . N(2) . 1.943(6) yes
Ni . N(3) . 1.956(5) yes
Ni . N(4) . 1.930(6) yes
N(1) . C(1) . 1.468(9) yes
N(2) . C(3) . 1.46(1) yes
N(2) . C(4) . 1.48(1) yes
N(3) . C(5) . 1.486(9) yes
N(3) . C(6) . 1.471(9) yes
N(3) . C(7) . 1.51(1) yes
N(4) . C(9) . 1.48(1) yes
C(1) . C(2) . 1.50(1) yes
C(2) . C(3) . 1.52(1) yes
C(4) . C(5) . 1.46(1) yes
C(7) . C(8) . 1.52(1) yes
C(8) . C(9) . 1.48(1) yes
