#------------------------------------------------------------------------------
#$Date: 2018-09-29 05:11:45 +0300 (Sat, 29 Sep 2018) $
#$Revision: 211234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/26/2242661.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_2242661
loop_
_publ_author_name
'Ohba, Shigeru'
'Tsuchimoto, Masanobu'
'Kurachi, Saeko'
_publ_section_title
;
 Investigation of solid-state photochemical nitro--nitrito linkage
 isomerization: crystal structures of
 trans-bis(ethylenediamine)(isothiocyanato)nitritocobalt(III)
 salts: thiocyanate, chloride monohydrate, and
 perchlorate--thiocyanate(0.75/0.25)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1526
_journal_page_last               1531
_journal_paper_doi               10.1107/S2056989018013634
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Co (C N S) (N O2) (C2 H8 N2)2] (C N S)'
_chemical_formula_moiety         'C5 H16 Co N6 O2 S +, C N S -'
_chemical_formula_structural     '[Co (N O2) (C N S) (C2 H8 N2)2]  (C N S)'
_chemical_formula_sum            'C6 H16 Co N7 O2 S2'
_chemical_formula_weight         341.31
_chemical_name_systematic
;
trans-Bis(ethylenediamine)(isothiocyanato)nitritocobalt(III)
thiocyanate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.2599(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3222(7)
_cell_length_b                   16.0137(6)
_cell_length_c                   11.1284(4)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    299
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.54
_cell_volume                     2728.77(19)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008) and CAVITY (Ohashi et al.,
1981)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014  (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      299
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14627
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.911
_diffrn_reflns_theta_min         2.323
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  0.74299
_exptl_absorpt_correction_T_min  0.66703
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      1.65(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.917
_refine_ls_extinction_coef       0.0080(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1131P)²+7.7542P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                2845
_reflns_number_total             3166
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7774sup1.cif
_cod_data_source_block           I
_cod_database_code               2242661
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.744
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.24789(3) 0.11825(3) 0.23306(4) 0.0283(2) Uani d 1 . .
S S2 0.16608(6) 0.13940(6) 0.59617(8) 0.0395(3) Uani d 1 . .
S S3 0.4182(2) 0.1460(3) 0.6750(5) 0.0699(8) Uani d 0.5 A -1
S S4 0.4754(2) 0.45097(14) 0.2044(3) 0.0701(8) Uani d 0.5 B -1
O O5 0.2530(4) 0.0509(3) 0.0120(4) 0.1008(17) Uani d 1 . .
O O6 0.3109(3) 0.1679(3) 0.0477(4) 0.0816(12) Uani d 1 . .
N N7 0.2733(2) 0.1111(2) 0.0787(3) 0.0404(7) Uani d 1 . .
N N8 0.2210(2) 0.12697(17) 0.3870(3) 0.0388(7) Uani d 1 . .
N N9 0.13307(19) 0.0704(2) 0.1463(3) 0.0403(6) Uani d 1 . .
H H9A 0.1308 0.0480 0.0720 0.048 Uiso calc 1 . .
H H9B 0.1223 0.0304 0.1943 0.048 Uiso calc 1 . .
N N10 0.19177(19) 0.22653(18) 0.1777(3) 0.0379(6) Uani d 1 . .
H H10A 0.1885 0.2544 0.2451 0.045 Uiso calc 1 . .
H H10B 0.2235 0.2566 0.1426 0.045 Uiso calc 1 . .
N N11 0.36443(17) 0.16416(19) 0.3219(3) 0.0379(6) Uani d 1 . .
H H11A 0.3784 0.2000 0.2710 0.045 Uiso calc 1 . .
H H11B 0.3649 0.1915 0.3918 0.045 Uiso calc 1 . .
N N12 0.30175(19) 0.00934(17) 0.2894(3) 0.0357(6) Uani d 1 . .
H H12A 0.2704 -0.0189 0.3271 0.043 Uiso calc 1 . .
H H12B 0.3027 -0.0199 0.2219 0.043 Uiso calc 1 . .
N N13 0.5878(6) 0.1646(14) 0.8455(16) 0.0699(8) Uani d 0.5 A -1
N N14 0.5058(18) 0.2805(4) 0.248(3) 0.061(3) Uani d 0.5 B -1
C C15 0.0661(3) 0.1389(3) 0.1234(5) 0.0552(11) Uani d 1 . .
H H15A 0.0121 0.1227 0.0568 0.066 Uiso calc 1 . .
H H15B 0.0538 0.1502 0.2012 0.066 Uiso calc 1 . .
C C16 0.1033(3) 0.2141(3) 0.0836(4) 0.0537(10) Uani d 1 . .
H H16A 0.1060 0.2062 -0.0013 0.064 Uiso calc 1 . .
H H16B 0.0672 0.2625 0.0819 0.064 Uiso calc 1 . .
C C17 0.4281(3) 0.0962(3) 0.3576(6) 0.0694(15) Uani d 1 . .
H H17A 0.4519 0.0880 0.2898 0.083 Uiso calc 1 . .
H H17B 0.4759 0.1117 0.4346 0.083 Uiso calc 1 . .
C C18 0.3910(3) 0.0202(3) 0.3795(7) 0.087(2) Uani d 1 . .
H H18A 0.3905 0.0197 0.4664 0.105 Uiso calc 1 . .
H H18B 0.4268 -0.0261 0.3706 0.105 Uiso calc 1 . .
C C19 0.1993(2) 0.13285(19) 0.4742(3) 0.0323(7) Uani d 1 . .
C C20 0.5197(4) 0.1522(7) 0.7695(10) 0.0699(8) Uani d 0.5 A -1
C C21 0.4903(12) 0.3510(3) 0.2317(12) 0.039(3) Uani d 0.5 B -1
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
N7 Co1 N8 179.03(13) ?
N7 Co1 N9 90.11(14) ?
N8 Co1 N9 89.61(14) ?
N7 Co1 N12 91.22(13) ?
N8 Co1 N12 89.72(12) ?
N9 Co1 N12 93.23(13) ?
N7 Co1 N11 90.05(14) ?
N8 Co1 N11 90.25(14) ?
N9 Co1 N11 178.80(13) ?
N12 Co1 N11 85.57(12) ?
N7 Co1 N10 89.64(13) ?
N8 Co1 N10 89.41(12) ?
N9 Co1 N10 85.84(13) ?
N12 Co1 N10 178.74(12) ?
N11 Co1 N10 95.35(12) ?
O5 N7 O6 119.3(4) n
O5 N7 Co1 120.6(3) ?
O6 N7 Co1 120.1(3) ?
C19 N8 Co1 175.5(3) ?
C15 N9 Co1 108.3(2) ?
C15 N9 H9A 110.0 ?
Co1 N9 H9A 110.0 ?
C15 N9 H9B 110.0 ?
Co1 N9 H9B 110.0 ?
H9A N9 H9B 108.4 ?
C16 N10 Co1 109.9(2) ?
C16 N10 H10A 109.7 ?
Co1 N10 H10A 109.7 ?
C16 N10 H10B 109.7 ?
Co1 N10 H10B 109.7 ?
H10A N10 H10B 108.2 ?
C17 N11 Co1 109.4(3) ?
C17 N11 H11A 109.8 ?
Co1 N11 H11A 109.8 ?
C17 N11 H11B 109.8 ?
Co1 N11 H11B 109.8 ?
H11A N11 H11B 108.2 ?
C18 N12 Co1 110.1(3) ?
C18 N12 H12A 109.6 ?
Co1 N12 H12A 109.6 ?
C18 N12 H12B 109.6 ?
Co1 N12 H12B 109.6 ?
H12A N12 H12B 108.2 ?
C16 C15 N9 107.1(3) ?
C16 C15 H15A 110.3 ?
N9 C15 H15A 110.3 ?
C16 C15 H15B 110.3 ?
N9 C15 H15B 110.3 ?
H15A C15 H15B 108.6 ?
N10 C16 C15 107.4(3) ?
N10 C16 H16A 110.2 ?
C15 C16 H16A 110.2 ?
N10 C16 H16B 110.2 ?
C15 C16 H16B 110.2 ?
H16A C16 H16B 108.5 ?
C18 C17 N11 112.3(4) ?
C18 C17 H17A 109.1 ?
N11 C17 H17A 109.1 ?
C18 C17 H17B 109.1 ?
N11 C17 H17B 109.1 ?
H17A C17 H17B 107.9 ?
C17 C18 N12 111.5(4) ?
C17 C18 H18A 109.3 ?
N12 C18 H18A 109.3 ?
C17 C18 H18B 109.3 ?
N12 C18 H18B 109.3 ?
H18A C18 H18B 108.0 ?
N8 C19 S2 178.4(4) ?
N13 C20 S3 170.7(13) ?
N14 C21 S4 175(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N7 1.905(3) n
Co1 N8 1.915(3) n
Co1 N9 1.944(3) n
Co1 N12 1.956(3) n
Co1 N11 1.958(3) n
Co1 N10 1.958(3) n
S2 C19 1.630(3) ?
S3 C20 1.629(3) ?
S4 C21 1.633(3) ?
O5 N7 1.191(5) n
O6 N7 1.212(4) n
N8 C19 1.146(5) ?
N9 C15 1.507(5) ?
N9 H9A 0.8900 ?
N9 H9B 0.8900 ?
N10 C16 1.474(5) ?
N10 H10A 0.8900 ?
N10 H10B 0.8900 ?
N11 C17 1.462(6) ?
N11 H11A 0.8900 ?
N11 H11B 0.8900 ?
N12 C18 1.466(6) ?
N12 H12A 0.8900 ?
N12 H12B 0.8900 ?
N13 C20 1.157(4) ?
N14 C21 1.156(4) ?
C15 C16 1.484(6) ?
C15 H15A 0.9700 ?
C15 H15B 0.9700 ?
C16 H16A 0.9700 ?
C16 H16B 0.9700 ?
C17 C18 1.417(8) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 H18A 0.9700 ?
C18 H18B 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N9 H9A O5 . 0.89 2.31 2.861(5) 119.9
N9 H9B S4 3_445 0.89 2.75 3.443(4) 135.5
N9 H9B S4 4_545 0.89 2.58 3.404(4) 153.7
N10 H10A S3 7_556 0.89 2.73 3.480(7) 143.0
N10 H10A N13 8_455 0.89 2.63 3.41(2) 146.5
N10 H10B O6 . 0.89 2.49 2.950(5) 112.5
N10 H10B O6 7 0.89 2.33 3.013(4) 133.2
N11 H11A O6 . 0.89 2.40 2.869(5) 113.2
N11 H11A N14 . 0.89 2.53 3.28(3) 142.3
N11 H11A N14 2_655 0.89 2.36 3.12(2) 143.2
N11 H11B S2 7_556 0.89 2.77 3.360(3) 125.2
N12 H12A O5 6_556 0.89 2.23 3.011(4) 146.0
N12 H12B O5 . 0.89 2.47 2.984(5) 117.4
C15 H15A S2 2 0.97 2.83 3.731(4) 155.1
C18 H18B S3 6 0.97 2.87 3.627(8) 135.7
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
Co1 N9 C15 C16 40.7(4) ?
Co1 N10 C16 C15 36.7(4) ?
N9 C15 C16 N10 -50.2(5) n
Co1 N11 C17 C18 -29.4(6) ?
N11 C17 C18 N12 37.6(8) n
Co1 N12 C18 C17 -27.4(7) ?
N10 Co1 N9 C15 -16.5(3) n
N9 Co1 N10 C16 -11.2(3) n
N12 Co1 N11 C17 10.8(3) n
N11 Co1 N12 C18 8.7(4) n
O5 N7 Co1 N9 -41.7(4) ?
O5 N7 Co1 N12 51.5(5) ?
O6 N7 Co1 N10 52.8(4) ?
O6 N7 Co1 N11 -42.6(4) ?

_cod_database_fobs_code 2242661
