#------------------------------------------------------------------------------
#$Date: 2016-02-19 15:29:56 +0100 (vie 19 de feb de 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/57/2005793.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_2005793
loop_
_publ_author_name
'Kožíšek, J.'
'Paulus, H.'
'Danková, M.'
'Hvastijová, M.'
_publ_section_title
trans-Bis(dicyanamido-N)tetrakis(4-methylimidazole-N¹)nickel(II)
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              3019
_journal_page_last               3020
_journal_paper_doi               10.1107/S0108270196010311
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ni (C2 N3)2 (C4 H6 N2)4]'
_chemical_formula_moiety         'C20 H24 N14 Ni'
_chemical_formula_sum            'C20 H24 N14 Ni'
_chemical_formula_weight         519.24
_chemical_name_systematic
;
Bis(dicyanamide)tetrakis(4-methylimidazole) nickel(II) complex,
C₂₀H₂₄N₁₄Ni₁
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                107.85(2)
_cell_angle_beta                 93.67(2)
_cell_angle_gamma                104.74(2)
_cell_formula_units_Z            2
_cell_length_a                   9.448(3)
_cell_length_b                   9.918(3)
_cell_length_c                   15.173(5)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      16.9
_cell_volume                     1293.1(7)
_computing_molecular_graphics    'ORTEPII (Johnson, 1971)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE STADI4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8280
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_obs          0.0370
_refine_ls_shift/esd_max         0.042
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0392P)²+0.4257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1118
_refine_ls_wR_factor_obs         0.0872
_reflns_number_observed          5669
_reflns_number_total             7523
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1201.cif
_cod_data_source_block           KOZ3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.4257P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.4257P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2005793
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
Ni1 1 0 0 0 0.03853(9) Uani d S Ni
N2 1 -0.0151(2) 0.1403(2) 0.13140(11) 0.0465(4) Uani d . N
C3 1 0.0319(3) 0.1341(3) 0.2170(2) 0.0663(6) Uani d . C
H3 1 0.0712(3) 0.0615(3) 0.2260(2) 0.080 Uiso calc R H
C4 1 0.0130(3) 0.2488(3) 0.2865(2) 0.0679(7) Uani d . C
C5 1 0.0476(4) 0.2934(5) 0.3908(2) 0.118(2) Uani d G C
H5A 1 -0.0165(24) 0.3464(29) 0.4187(6) 0.141 Uiso calc R H
H5B 1 0.1459(23) 0.3532(28) 0.4111(5) 0.141 Uiso calc R H
H5C 1 0.0351(29) 0.2086(18) 0.4082(5) 0.141 Uiso calc R H
N6 1 -0.0472(2) 0.3254(2) 0.24223(14) 0.0663(5) Uani d . N
H6 1 -0.0710(2) 0.4047(2) 0.26903(14) 0.080 Uiso calc R H
C7 1 -0.0636(3) 0.2563(2) 0.1491(2) 0.0580(5) Uani d . C
H7 1 -0.1038(3) 0.2870(2) 0.1038(2) 0.070 Uiso calc R H
N8 1 0.2275(2) 0.0438(2) 0.04806(12) 0.0456(4) Uani d . N
C9 1 0.3003(2) -0.0279(2) 0.0917(2) 0.0540(5) Uani d . C
H9 1 0.2557(2) -0.1178(2) 0.0993(2) 0.065 Uiso calc R H
C10 1 0.4450(2) 0.0490(2) 0.1220(2) 0.0537(5) Uani d . C
C11 1 0.5694(3) 0.0229(4) 0.1730(2) 0.0790(8) Uani d G C
H11A 1 0.5381(8) -0.0669(17) 0.1813(12) 0.095 Uiso calc R H
H11B 1 0.6008(15) 0.0959(17) 0.2302(11) 0.095 Uiso calc R H
H11C 1 0.6459(15) 0.0238(21) 0.1390(9) 0.095 Uiso calc R H
N12 1 0.4613(2) 0.1710(2) 0.09562(14) 0.0607(5) Uani d . N
H12 1 0.5422(2) 0.2409(2) 0.10523(14) 0.073 Uiso calc R H
C13 1 0.3303(2) 0.1637(2) 0.0522(2) 0.0566(5) Uani d . C
H13 1 0.3141(2) 0.2349(2) 0.0280(2) 0.068 Uiso calc R H
N14 1 -0.0475(2) -0.1809(2) 0.05014(13) 0.0508(4) Uani d . N
C15 1 -0.0767(2) -0.2677(2) 0.08593(14) 0.0464(4) Uani d . C
N16 1 -0.0921(2) -0.3612(3) 0.1316(2) 0.0783(7) Uani d . N
C17 1 -0.2168(3) -0.4587(2) 0.1235(2) 0.0567(5) Uani d . C
N18 1 -0.3175(3) -0.5503(3) 0.1215(2) 0.0937(8) Uani d . N
Ni19 1 0.5000 0 0.5000 0.03534(8) Uani d S Ni
N20 1 0.3782(2) -0.1425(2) 0.36880(11) 0.0426(3) Uani d . N
C21 1 0.4243(2) -0.2377(2) 0.29782(15) 0.0509(5) Uani d . C
H21 1 0.5205(2) -0.2451(2) 0.29809(15) 0.061 Uiso calc R H
C22 1 0.3106(3) -0.3190(2) 0.2275(2) 0.0566(5) Uani d . C
C23 1 0.3009(4) -0.4357(4) 0.1361(2) 0.0986(11) Uani d G C
H23A 1 0.3967(18) -0.4475(18) 0.1280(8) 0.118 Uiso calc R H
H23B 1 0.2645(25) -0.4075(13) 0.0866(9) 0.118 Uiso calc R H
H23C 1 0.2354(23) -0.5268(18) 0.1353(6) 0.118 Uiso calc R H
N24 1 0.1921(2) -0.2723(2) 0.25571(13) 0.0589(5) Uani d . N
H24 1 0.1040(2) -0.3047(2) 0.22468(13) 0.071 Uiso calc R H
C25 1 0.2368(2) -0.1668(2) 0.3404(2) 0.0542(5) Uani d . C
H25 1 0.1758(2) -0.1176(2) 0.3745(2) 0.065 Uiso calc R H
N26 1 0.5393(2) 0.1796(2) 0.45108(12) 0.0454(4) Uani d . N
C27 1 0.4417(3) 0.2218(3) 0.4018(2) 0.0571(5) Uani d . C
H27 1 0.3408(3) 0.1736(3) 0.3849(2) 0.068 Uiso calc R H
C28 1 0.5119(3) 0.3427(3) 0.3812(2) 0.0596(6) Uani d . C
C29 1 0.4585(4) 0.4331(4) 0.3313(2) 0.0943(11) Uani d G C
H29A 1 0.5186(19) 0.4466(21) 0.2860(14) 0.113 Uiso calc R H
H29B 1 0.4630(23) 0.5256(19) 0.3745(8) 0.113 Uiso calc R H
H29C 1 0.3603(20) 0.3839(15) 0.3019(14) 0.113 Uiso calc R H
N30 1 0.6561(2) 0.3741(2) 0.4180(2) 0.0664(5) Uani d . N
H30 1 0.7278(2) 0.4456(2) 0.4154(2) 0.080 Uiso calc R H
C31 1 0.6674(3) 0.2745(2) 0.4591(2) 0.0622(6) Uani d . C
H31 1 0.7556(3) 0.2733(2) 0.4895(2) 0.075 Uiso calc R H
N32 1 0.6976(2) -0.0440(2) 0.45719(13) 0.0492(4) Uani d . N
C33 1 0.7844(2) -0.0990(2) 0.4283(2) 0.0479(4) Uani d . C
N34 1 0.8906(2) -0.1515(2) 0.3949(2) 0.0857(8) Uani d . N
C35 1 0.8835(2) -0.2888(2) 0.3804(2) 0.0523(5) Uani d . C
N36 1 0.8910(3) -0.4064(2) 0.3662(2) 0.0692(6) Uani d . N
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Ni1 N2 . 2 180.0 ?
N2 Ni1 N14 . . 89.81(7) yes
N2 Ni1 N14 2 . 90.19(7) ?
N2 Ni1 N14 . 2 90.19(7) ?
N2 Ni1 N14 2 2 89.81(7) ?
N14 Ni1 N14 . 2 180.0 ?
N2 Ni1 N8 . . 87.89(7) yes
N2 Ni1 N8 2 . 92.11(7) ?
N14 Ni1 N8 . . 89.25(7) yes
N14 Ni1 N8 2 . 90.75(7) ?
N2 Ni1 N8 . 2 92.11(7) ?
N2 Ni1 N8 2 2 87.89(7) ?
N14 Ni1 N8 . 2 90.75(7) ?
N14 Ni1 N8 2 2 89.25(7) ?
N8 Ni1 N8 . 2 180.0 ?
C7 N2 C3 . . 105.8(2) ?
C7 N2 Ni1 . . 127.2(2) ?
C3 N2 Ni1 . . 126.92(14) ?
C4 C3 N2 . . 110.2(2) ?
C4 C3 H3 . . 124.9(2) ?
N2 C3 H3 . . 124.90(12) ?
C3 C4 N6 . . 105.1(2) ?
C3 C4 C5 . . 131.4(3) ?
N6 C4 C5 . . 123.5(2) ?
C4 C5 H5A . . 109.5(2) ?
C4 C5 H5B . . 109.5(2) ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5(2) ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C7 N6 C4 . . 108.4(2) ?
C7 N6 H6 . . 125.81(14) ?
C4 N6 H6 . . 125.80(13) ?
N2 C7 N6 . . 110.5(2) ?
N2 C7 H7 . . 124.73(13) ?
N6 C7 H7 . . 124.73(14) ?
C13 N8 C9 . . 104.1(2) ?
C13 N8 Ni1 . . 124.3(2) ?
C9 N8 Ni1 . . 131.07(13) ?
C10 C9 N8 . . 111.5(2) ?
C10 C9 H9 . . 124.24(14) ?
N8 C9 H9 . . 124.24(11) ?
C9 C10 N12 . . 104.1(2) ?
C9 C10 C11 . . 133.3(2) ?
N12 C10 C11 . . 122.6(2) ?
C10 C11 H11A . . 109.47(14) ?
C10 C11 H11B . . 109.5(2) ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.47(14) ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 N12 C10 . . 108.5(2) ?
C13 N12 H12 . . 125.75(12) ?
C10 N12 H12 . . 125.74(12) ?
N8 C13 N12 . . 111.7(2) ?
N8 C13 H13 . . 124.13(13) ?
N12 C13 H13 . . 124.12(12) ?
C15 N14 Ni1 . . 172.2(2) yes
N14 C15 N16 . . 172.6(2) yes
C17 N16 C15 . . 122.0(2) yes
N18 C17 N16 . . 172.8(3) yes
N26 Ni19 N26 2_656 . 179.9990(10) ?
N26 Ni19 N20 2_656 . 89.29(7) ?
N26 Ni19 N20 . . 90.71(7) yes
N26 Ni19 N20 2_656 2_656 90.71(7) ?
N26 Ni19 N20 . 2_656 89.29(7) ?
N20 Ni19 N20 . 2_656 180.0 ?
N26 Ni19 N32 2_656 2_656 90.62(7) ?
N26 Ni19 N32 . 2_656 89.38(7) ?
N20 Ni19 N32 . 2_656 89.33(7) ?
N20 Ni19 N32 2_656 2_656 90.67(7) ?
N26 Ni19 N32 2_656 . 89.38(7) ?
N26 Ni19 N32 . . 90.62(7) yes
N20 Ni19 N32 . . 90.67(7) yes
N20 Ni19 N32 2_656 . 89.33(7) ?
N32 Ni19 N32 2_656 . 180.0 ?
C25 N20 C21 . . 105.1(2) ?
C25 N20 Ni19 . . 126.54(14) ?
C21 N20 Ni19 . . 128.23(13) ?
C22 C21 N20 . . 110.6(2) ?
C22 C21 H21 . . 124.69(14) ?
N20 C21 H21 . . 124.69(11) ?
C21 C22 N24 . . 105.1(2) ?
C21 C22 C23 . . 132.3(3) ?
N24 C22 C23 . . 122.6(2) ?
C22 C23 H23A . . 109.5(2) ?
C22 C23 H23B . . 109.5(2) ?
H23A C23 H23B . . 109.5 ?
C22 C23 H23C . . 109.5(2) ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C25 N24 C22 . . 108.2(2) ?
C25 N24 H24 . . 125.92(13) ?
C22 N24 H24 . . 125.92(12) ?
N20 C25 N24 . . 111.0(2) ?
N20 C25 H25 . . 124.48(12) ?
N24 C25 H25 . . 124.48(13) ?
C31 N26 C27 . . 104.8(2) ?
C31 N26 Ni19 . . 126.0(2) ?
C27 N26 Ni19 . . 129.20(14) ?
C28 C27 N26 . . 110.9(2) ?
C28 C27 H27 . . 124.54(15) ?
N26 C27 H27 . . 124.53(12) ?
C27 C28 N30 . . 104.6(2) ?
C27 C28 C29 . . 132.6(3) ?
N30 C28 C29 . . 122.8(2) ?
C28 C29 H29A . . 109.5(2) ?
C28 C29 H29B . . 109.5(2) ?
H29A C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5(2) ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C31 N30 C28 . . 108.3(2) ?
C31 N30 H30 . . 125.85(14) ?
C28 N30 H30 . . 125.85(12) ?
N26 C31 N30 . . 111.4(2) ?
N26 C31 H31 . . 124.31(13) ?
N30 C31 H31 . . 124.31(14) ?
C33 N32 Ni19 . . 164.8(2) yes
N32 C33 N34 . . 175.2(2) yes
C35 N34 C33 . . 120.6(2) yes
N36 C35 N34 . . 173.5(2) yes
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
Ni1 N2 . 2.090(2) yes
Ni1 N2 2 2.090(2) ?
Ni1 N14 . 2.114(2) yes
Ni1 N14 2 2.114(2) ?
Ni1 N8 . 2.115(2) yes
Ni1 N8 2 2.115(2) ?
N2 C7 . 1.304(3) ?
N2 C3 . 1.370(3) ?
C3 C4 . 1.353(3) ?
C3 H3 . 0.93 ?
C4 N6 . 1.355(3) ?
C4 C5 . 1.497(4) ?
C5 H5A . 0.94(2) ?
C5 H5B . 0.94(2) ?
C5 H5C . 0.94(2) ?
N6 C7 . 1.347(3) ?
N6 H6 . 0.86 ?
C7 H7 . 0.93 ?
N8 C13 . 1.311(2) ?
N8 C9 . 1.376(3) ?
C9 C10 . 1.355(3) ?
C9 H9 . 0.93 ?
C10 N12 . 1.363(3) ?
C10 C11 . 1.486(3) ?
C11 H11A . 0.914(15) ?
C11 H11B . 0.914(15) ?
C11 H11C . 0.914(15) ?
N12 C13 . 1.339(3) ?
N12 H12 . 0.86 ?
C13 H13 . 0.93 ?
N14 C15 . 1.140(2) yes
C15 N16 . 1.304(3) yes
N16 C17 . 1.291(3) yes
C17 N18 . 1.127(3) yes
Ni19 N26 2_656 2.090(2) ?
Ni19 N26 . 2.090(2) yes
Ni19 N20 . 2.107(2) yes
Ni19 N20 2_656 2.107(2) ?
Ni19 N32 2_656 2.120(2) ?
Ni19 N32 . 2.120(2) yes
N20 C25 . 1.314(3) ?
N20 C21 . 1.373(3) ?
C21 C22 . 1.352(3) ?
C21 H21 . 0.93 ?
C22 N24 . 1.362(3) ?
C22 C23 . 1.489(3) ?
C23 H23A . 0.95(2) ?
C23 H23B . 0.95(2) ?
C23 H23C . 0.95(2) ?
N24 C25 . 1.344(3) ?
N24 H24 . 0.86 ?
C25 H25 . 0.93 ?
N26 C31 . 1.303(3) ?
N26 C27 . 1.373(3) ?
C27 C28 . 1.352(3) ?
C27 H27 . 0.93 ?
C28 N30 . 1.358(3) ?
C28 C29 . 1.493(3) ?
C29 H29A . 0.94(2) ?
C29 H29B . 0.94(2) ?
C29 H29C . 0.94(2) ?
N30 C31 . 1.342(3) ?
N30 H30 . 0.86 ?
C31 H31 . 0.93 ?
N32 C33 . 1.135(2) yes
C33 N34 . 1.305(3) yes
N34 C35 . 1.294(3) yes
C35 N36 . 1.141(3) yes
