#------------------------------------------------------------------------------
#$Date: 2017-05-30 17:58:23 +0300 (Tue, 30 May 2017) $
#$Revision: 197043 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/72/2007209.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_2007209
loop_
_publ_author_name
'Choi, Ki Young'
'Kim, Dong Won'
'Kim, Kyung-Han'
'Oh, Mi-Ran'
'Suh, Il-Hwan'
_publ_section_title
;
 Co-Crystallized (Macrocyclic
 tetraamine)bis(thiocyanato-N)nickel(II) Complexes
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              627
_journal_page_last               628
_journal_paper_doi               10.1107/S0108270197017368
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          'Ni(NCS)~2~(C14 H32 N4)2 , C2 H3 N'
_chemical_formula_moiety         'C16 H32 N6 Ni S2 , C2 H3 N'
_chemical_formula_sum            'C18 H35 N7 Ni S2'
_chemical_formula_weight         472.34
_chemical_name_systematic
;
 ?
;
_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                90.81(2)
_cell_angle_beta                 91.18(2)
_cell_angle_gamma                104.910(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9990(10)
_cell_length_b                   13.867(2)
_cell_length_c                   8.911(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      11.35
_cell_volume                     1193.5(6)
_computing_cell_refinement       SDP
_computing_data_collection       SDP_(Frenz,_1985)
_computing_data_reduction        SDP
_computing_molecular_graphics
ORTEP_(Johnson,_1976)_in_NRCVAX_(Gabe_et_al.,_1989)
_computing_publication_material  NRCVAX
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       ω/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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0650
_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       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4374
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block_cut_from_a_larger_crystal
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.39
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.270
_refine_ls_goodness_of_fit_obs   1.438
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.270
_refine_ls_restrained_S_obs      1.438
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_obs          .0583
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.02P)²+0.40P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1073
_refine_ls_wR_factor_obs         .0936
_reflns_number_observed          2576
_reflns_number_total             4183
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm1168.cif
_cod_data_source_block           real5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.02P)^2^+0.40P] 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^)+(0.02P)^2^+0.40P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2017-05-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H70 N14 Ni2 S4'
_cod_original_formula_weight         944.69
_cod_original_formula_moiety         '2(C16 H32 N6 Ni S2) , 2(C2 H3 N)'
_cod_original_formula_iupac          '2[Ni(NCS)~2~(C14 H32 N4)2] , 2C2 H3 N'
_cod_original_formula_units_Z            1
_cod_database_code               2007209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ni1 .5000 .0000 .0000 .0424(2) Uani d S 1 . Ni
S1 .1555(2) -.14683(12) .3641(2) .0900(6) Uani d . 1 . S
N11 .3370(4) -.0677(3) .1410(5) .0592(12) Uani d . 1 . N
N12 .6193(4) .0580(3) .1861(4) .0513(10) Uani d . 1 . N
HN12 .7010(4) .0965(3) .1530(4) .062 Uiso calc R 1 . H
N13 .4220(4) .1250(3) -.0369(4) .0467(10) Uani d . 1 . N
HN13 .4915(4) .1683(3) -.0846(4) .056 Uiso calc R 1 . H
C11 .2604(5) -.1015(3) .2311(6) .0491(13) Uani d . 1 . C
C12 .5601(5) .1218(4) .2850(6) .067(2) Uani d . 1 . C
H12A .6257(5) .1487(4) .3663(6) .080 Uiso calc R 1 . H
H12B .4765(5) .0816(4) .3285(6) .080 Uiso calc R 1 . H
C13 .5261(5) .2077(4) .2005(6) .0614(15) Uani d . 1 . C
H13A .5151(5) .2572(4) .2739(6) .074 Uiso calc R 1 . H
H13B .6052(5) .2385(4) .1409(6) .074 Uiso calc R 1 . H
C14 .3986(5) .1825(3) .0977(5) .0523(13) Uani d . 1 . C
H14 .3227(5) .1400(3) .1530(5) .063 Uiso calc R 1 . H
C15 .3076(6) .0981(4) -.1523(6) .0628(14) Uani d . 1 . C
H15 .3039(6) .1588(4) -.2055(6) .075 Uiso calc R 1 . H
C16 .3499(6) .0266(4) -.2639(6) .067(2) Uani d . 1 . C
H16A .2754(6) .0021(4) -.3373(6) .081 Uiso calc R 1 . H
H16B .4309(6) .0623(4) -.3169(6) .081 Uiso calc R 1 . H
C17 .3567(6) .2778(4) .0574(6) .072(2) Uani d . 1 . C
H17A .2760(6) .2611(4) -.0076(6) .109 Uiso calc R 1 . H
H17B .4312(6) .3223(4) .0072(6) .109 Uiso calc R 1 . H
H17C .3365(6) .3097(4) .1474(6) .109 Uiso calc R 1 . H
C18 .1687(5) .0546(4) -.0876(7) .079(2) Uani d . 1 . C
H18A .1471(5) .1020(4) -.0188(7) .118 Uiso calc R 1 . H
H18B .1701(5) -.0053(4) -.0355(7) .118 Uiso calc R 1 . H
H18C .0998(5) .0391(4) -.1670(7) .118 Uiso calc R 1 . H
Ni2 1.0000 .5000 .5000 .0430(3) Uani d S 1 . Ni
S2 .9388(2) .23283(10) .1304(2) .0721(5) Uani d . 1 . S
N21 .9808(4) .3697(3) .3676(5) .0632(12) Uani d . 1 . N
N22 .8950(4) .4116(3) .6666(4) .0546(11) Uani d . 1 . N
HN22 .8848(4) .3472(3) .6361(4) .066 Uiso calc R 1 . H
N23 1.1941(4) .4898(3) .5712(5) .0590(11) Uani d . 1 . N
HN23 1.2037(4) .4305(3) .5342(5) .071 Uiso calc R 1 . H
C21 .9638(5) .3120(3) .2720(5) .0434(12) Uani d . 1 . C
C22 .9681(6) .4236(4) .8127(6) .078(2) Uani d . 1 . C
H22A .9142(6) .3767(4) .8821(6) .094 Uiso calc R 1 . H
H22B .9757(6) .4905(4) .8520(6) .094 Uiso calc R 1 . H
C23 1.1092(6) .4071(5) .8040(7) .101(2) Uani d . 1 . C
H23A 1.1019(6) .3462(5) .7461(7) .121 Uiso calc R 1 . H
H23B 1.1396(6) .3960(5) .9049(7) .121 Uiso calc R 1 . H
C24 1.2216(6) .4894(6) .7362(8) .106(3) Uani d . 1 . C
H24 1.2052(6) .5518(6) .7747(8) .127 Uiso calc R 1 . H
C25 1.2937(5) .5681(4) .4917(6) .074(2) Uani d . 1 . C
H25A 1.3838(5) .5539(4) .4937(6) .089 Uiso calc R 1 . H
H25B 1.3028(5) .6321(4) .5417(6) .089 Uiso calc R 1 . H
C26 1.2450(6) .5728(4) .3295(7) .073(2) Uani d . 1 . C
H26 1.2384(6) .5080(4) .2806(7) .087 Uiso calc R 1 . H
C27 1.3482(6) .6514(5) .2460(8) .124(3) Uani d . 1 . C
H27A 1.3160(6) .6533(5) .1442(8) .186 Uiso calc R 1 . H
H27B 1.4361(6) .6353(5) .2469(8) .186 Uiso calc R 1 . H
H27C 1.3583(6) .7153(5) .2940(8) .186 Uiso calc R 1 . H
C28 1.3550(8) .4921(6) .7832(9) .156(4) Uani d . 1 . C
H28A 1.4189(8) .5459(6) .7353(9) .234 Uiso calc R 1 . H
H28B 1.3753(8) .4301(6) .7569(9) .234 Uiso calc R 1 . H
H28C 1.3637(8) .5023(6) .8901(9) .234 Uiso calc R 1 . H
N .3142(8) .2871(6) .4890(9) .135(3) Uani d . 1 . N
C1 .2361(8) .2157(7) .4603(8) .089(2) Uani d . 1 . C
C2 .1346(7) .1257(5) .4206(8) .097(2) Uani d . 1 . C
H2A .074(3) .1058(18) .5029(19) .145 Uiso calc R 1 . H
H2B .1798(7) .0742(10) .398(5) .145 Uiso calc R 1 . H
H2C .082(3) .1366(10) .334(3) .145 Uiso calc R 1 . H
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'
S S 0.1246 0.1234 '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
N12 Ni1 N12 . 2_655 180.0 ?
N12 Ni1 N13 . . 96.03(14) y
N12 Ni1 N13 2_655 . 83.97(14) ?
N12 Ni1 N13 . 2_655 83.97(14) ?
N12 Ni1 N13 2_655 2_655 96.03(14) ?
N13 Ni1 N13 . 2_655 180.0 ?
N12 Ni1 N11 . 2_655 90.6(2) ?
N12 Ni1 N11 2_655 2_655 89.4(2) ?
N13 Ni1 N11 . 2_655 86.68(15) ?
N13 Ni1 N11 2_655 2_655 93.32(15) ?
N12 Ni1 N11 . . 89.4(2) y
N12 Ni1 N11 2_655 . 90.6(2) ?
N13 Ni1 N11 . . 93.32(15) y
N13 Ni1 N11 2_655 . 86.68(15) ?
N11 Ni1 N11 2_655 . 180.0 ?
C11 N11 Ni1 . . 171.8(4) ?
C16 N12 C12 2_655 . 113.1(4) ?
C16 N12 Ni1 2_655 . 106.6(3) ?
C12 N12 Ni1 . . 115.1(3) ?
C14 N13 C15 . . 117.1(4) ?
C14 N13 Ni1 . . 117.2(3) ?
C15 N13 Ni1 . . 108.9(3) ?
N11 C11 S1 . . 177.8(5) y
N12 C12 C13 . . 112.0(4) ?
C14 C13 C12 . . 117.1(4) ?
N13 C14 C13 . . 110.7(4) ?
N13 C14 C17 . . 112.7(4) ?
C13 C14 C17 . . 110.1(4) ?
N13 C15 C18 . . 113.5(4) ?
N13 C15 C16 . . 105.8(4) ?
C18 C15 C16 . . 112.7(4) ?
N12 C16 C15 2_655 . 110.9(4) ?
N22 Ni2 N22 2_766 . 180.0 ?
N22 Ni2 N23 2_766 2_766 95.1(2) ?
N22 Ni2 N23 . 2_766 84.9(2) ?
N22 Ni2 N23 2_766 . 84.9(2) ?
N22 Ni2 N23 . . 95.1(2) y
N23 Ni2 N23 2_766 . 180.0 ?
N22 Ni2 N21 2_766 2_766 88.5(2) ?
N22 Ni2 N21 . 2_766 91.5(2) ?
N23 Ni2 N21 2_766 2_766 88.8(2) ?
N23 Ni2 N21 . 2_766 91.2(2) ?
N22 Ni2 N21 2_766 . 91.5(2) ?
N22 Ni2 N21 . . 88.5(2) y
N23 Ni2 N21 2_766 . 91.2(2) ?
N23 Ni2 N21 . . 88.8(2) y
N21 Ni2 N21 2_766 . 180.0 ?
C21 N21 Ni2 . . 165.1(4) ?
C22 N22 C26 . 2_766 114.4(4) ?
C22 N22 Ni2 . . 114.6(3) ?
C26 N22 Ni2 2_766 . 107.5(3) ?
C25 N23 C24 . . 114.2(4) ?
C25 N23 Ni2 . . 105.8(3) ?
C24 N23 Ni2 . . 117.4(3) ?
N21 C21 S2 . . 177.7(5) y
N22 C22 C23 . . 112.7(5) ?
C22 C23 C24 . . 117.3(6) ?
C28 C24 N23 . . 117.1(6) ?
C28 C24 C23 . . 115.0(6) ?
N23 C24 C23 . . 108.5(5) ?
N23 C25 C26 . . 110.2(4) ?
N22 C26 C27 2_766 . 114.5(5) ?
N22 C26 C25 2_766 . 107.1(4) ?
C27 C26 C25 . . 110.6(5) ?
N C1 C2 . . 178.4(9) ?
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 N11 . 2.108(4) y
Ni1 N12 . 2.051(4) y
Ni1 N12 2_655 2.051(4) ?
Ni1 N13 . 2.103(3) y
Ni1 N13 2_655 2.103(3) ?
Ni1 N11 2_655 2.108(4) ?
S1 C11 . 1.623(5) y
N11 C11 . 1.141(5) y
N12 C16 2_655 1.468(6) ?
N12 C12 . 1.476(6) ?
N13 C14 . 1.487(5) ?
N13 C15 . 1.492(6) ?
C12 C13 . 1.524(6) ?
C13 C14 . 1.517(6) ?
C14 C17 . 1.530(6) ?
C15 C18 . 1.495(7) ?
C15 C16 . 1.535(6) ?
C16 N12 2_655 1.468(6) ?
Ni2 N21 . 2.109(4) y
Ni2 N22 2_766 2.064(4) ?
Ni2 N22 . 2.064(4) y
Ni2 N23 2_766 2.070(4) ?
Ni2 N23 . 2.070(4) y
Ni2 N21 2_766 2.109(4) ?
S2 C21 . 1.633(5) y
N21 C21 . 1.140(5) y
N22 C22 . 1.466(6) ?
N22 C26 2_766 1.471(6) ?
N23 C25 . 1.472(6) ?
N23 C24 . 1.490(7) ?
C22 C23 . 1.490(7) ?
C23 C24 . 1.522(8) ?
C24 C28 . 1.381(8) ?
C25 C26 . 1.524(7) ?
C26 N22 2_766 1.471(6) ?
C26 C27 . 1.510(7) ?
N C1 . 1.115(8) ?
C1 C2 . 1.425(9) ?
