#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/77/1507780.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_1507780
loop_
_publ_author_name
'Hatzipanayioti, D'
'Veneris, A'
'Parsons, S'
_publ_section_title
;
 Synthesis and spectroscopic investigation of new nickel(II) complexes
 with the open chain asymmetric tetraamine 1,4,7,11-tetraazaundecane:
 Crystal structure of the square-planar complex
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              2857
_journal_page_last               2861
_journal_paper_doi               10.1016/j.ica.2007.01.019
_journal_volume                  360
_journal_year                    2007
_chemical_formula_moiety         '[Ni(C7H20N4)](ClO4)2'
_chemical_formula_sum            'C7 H20 Cl2 N4 Ni O8'
_chemical_formula_weight         417.88
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.550(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9355(8)
_cell_length_b                   14.1122(11)
_cell_length_c                   10.9630(9)
_cell_measurement_reflns_used    5136
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2
_cell_volume                     1537.1(2)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_molecular_graphics    XP
_computing_publication_material  'XCIF, PLATON'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'Omega and phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs scaled by 0.71'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1072P)²+2.4751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                2160
_reflns_number_total             2701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ex6001.cif
_cod_data_source_block           ex6001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1507780
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
Ni1 Ni 0.25269(11) 0.11658(5) 0.72948(8) 0.0395(3) Uani 1 1 d .
N1 N 0.3549(7) 0.0632(4) 0.8597(6) 0.0477(17) Uani 1 1 d .
H1A H 0.3242 0.0861 0.9329 0.057 Uiso 1 1 calc R
H1B H 0.3447 -0.0016 0.8598 0.057 Uiso 1 1 calc R
C2 C 0.4992(10) 0.0875(7) 0.8459(9) 0.059(3) Uani 1 1 d .
H2A H 0.5555 0.0391 0.8872 0.071 Uiso 1 1 calc R
H2B H 0.5176 0.1495 0.8849 0.071 Uiso 1 1 calc R
C3 C 0.5352(8) 0.0922(6) 0.7112(9) 0.050(2) Uani 1 1 d .
H3A H 0.6262 0.1191 0.6997 0.060 Uiso 1 1 calc R
H3B H 0.5309 0.0287 0.6728 0.060 Uiso 1 1 calc R
N4 N 0.4287(7) 0.1566(5) 0.6601(6) 0.0497(18) Uani 1 1 d .
H4 H 0.4467 0.2168 0.6908 0.060 Uiso 1 1 calc R
C5 C 0.4217(12) 0.1657(8) 0.5299(10) 0.070(3) Uani 1 1 d .
H5A H 0.4294 0.1031 0.4899 0.084 Uiso 1 1 calc R
H5B H 0.4941 0.2075 0.4997 0.084 Uiso 1 1 calc R
C6 C 0.2869(9) 0.2083(7) 0.5067(8) 0.055(2) Uani 1 1 d .
H6A H 0.2668 0.2080 0.4181 0.065 Uiso 1 1 calc R
H6B H 0.2861 0.2748 0.5353 0.065 Uiso 1 1 calc R
N7 N 0.1813(8) 0.1517(5) 0.5736(7) 0.056(2) Uani 1 1 d .
H7 H 0.1739 0.0952 0.5305 0.067 Uiso 1 1 calc R
C8 C 0.0550(10) 0.1923(7) 0.5661(11) 0.071(3) Uani 1 1 d .
H8A H 0.0270 0.1955 0.4793 0.086 Uiso 1 1 calc R
H8B H 0.0603 0.2581 0.5973 0.086 Uiso 1 1 calc R
C9 C -0.0545(9) 0.1377(6) 0.6387(9) 0.051(2) Uani 1 1 d .
H9A H -0.1434 0.1659 0.6194 0.061 Uiso 1 1 calc R
H9B H -0.0562 0.0712 0.6102 0.061 Uiso 1 1 calc R
C10 C -0.0351(8) 0.1380(5) 0.7740(9) 0.051(2) Uani 1 1 d .
H10A H -0.0226 0.2039 0.8030 0.062 Uiso 1 1 calc R
H10B H -0.1161 0.1117 0.8136 0.062 Uiso 1 1 calc R
N11 N 0.0826(7) 0.0813(5) 0.8076(7) 0.0493(17) Uani 1 1 d .
H11A H 0.0645 0.0190 0.7891 0.059 Uiso 1 1 calc R
H11B H 0.0946 0.0851 0.8908 0.059 Uiso 1 1 calc R
Cl1 Cl -0.2520(2) 0.13728(9) 0.33786(14) 0.0407(4) Uani 1 1 d G
O11 O -0.1276(5) 0.1278(3) 0.2772(7) 0.111(4) Uani 1 1 d G
O21 O -0.3575(6) 0.1327(3) 0.2521(6) 0.104(4) Uani 1 1 d G
O31 O -0.2562(6) 0.2252(2) 0.3987(3) 0.0614(16) Uani 1 1 d G
O41 O -0.2665(7) 0.0635(3) 0.4234(3) 0.094(3) Uani 1 1 d G
Cl2 Cl 0.20722(17) 0.11856(10) 0.17677(16) 0.0419(5) Uani 1 1 d G
O12 O 0.3405(4) 0.1243(3) 0.1293(5) 0.067(2) Uani 1 1 d G
O22 O 0.1617(4) 0.2109(3) 0.2090(4) 0.0548(14) Uani 1 1 d G
O32 O 0.2066(5) 0.0595(3) 0.2822(4) 0.0694(18) Uani 1 1 d G
O42 O 0.1201(5) 0.0795(3) 0.0865(4) 0.0689(19) Uani 1 1 d G
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 Ni1 N7 165.2(3)
N1 Ni1 N11 91.6(3)
N7 Ni1 N11 98.2(3)
N1 Ni1 N4 86.3(3)
N7 Ni1 N4 84.5(3)
N11 Ni1 N4 176.3(3)
C2 N1 Ni1 110.0(5)
N1 C2 C3 110.2(7)
N4 C3 C2 102.5(7)
C5 N4 C3 116.9(8)
C5 N4 Ni1 111.7(7)
C3 N4 Ni1 107.7(5)
N4 C5 C6 104.0(8)
C5 C6 N7 109.3(7)
C8 N7 C6 112.7(7)
C8 N7 Ni1 119.4(8)
C6 N7 Ni1 108.5(5)
N7 C8 C9 113.7(8)
C10 C9 C8 115.0(8)
N11 C10 C9 110.1(8)
C10 N11 Ni1 116.1(6)
O21 Cl1 O31 109.4
O21 Cl1 O41 109.3
O31 Cl1 O41 109.4
O21 Cl1 O11 109.3
O31 Cl1 O11 109.7
O41 Cl1 O11 109.8
O42 Cl2 O32 109.3
O42 Cl2 O22 109.6
O32 Cl2 O22 109.3
O42 Cl2 O12 109.2
O32 Cl2 O12 109.9
O22 Cl2 O12 109.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 N1 1.900(7)
Ni1 N7 1.910(8)
Ni1 N11 1.966(7)
Ni1 N4 1.996(8)
N1 C2 1.483(12)
C2 C3 1.525(14)
C3 N4 1.499(10)
N4 C5 1.434(13)
C5 C6 1.488(14)
C6 N7 1.514(11)
N7 C8 1.381(12)
C8 C9 1.558(14)
C9 C10 1.494(13)
C10 N11 1.462(11)
Cl1 O21 1.403(3)
Cl1 O31 1.409(3)
Cl1 O41 1.410(3)
Cl1 O11 1.415(3)
Cl2 O42 1.420(3)
Cl2 O32 1.425(3)
Cl2 O22 1.426(3)
Cl2 O12 1.430(3)
