#------------------------------------------------------------------------------
#$Date: 2017-07-25 12:49:09 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/22/2242229.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_2242229
loop_
_publ_author_name
'Suckert, Stefan'
'Werner, Julia'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 bis(acetonitrile-κN)bis(4-benzoylpyridine-κN)bis(thiocyanato-κN)cobalt(II)
;
_journal_coeditor_code           WM5365
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              365
_journal_page_last               368
_journal_paper_doi               10.1107/S2056989017002201
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Co (N C S)2 (C2 H3 N)2 (C12 H9 N O)2]'
_chemical_formula_moiety         'C30 H24 Co N6 O2 S2'
_chemical_formula_sum            'C30 H24 Co N6 O2 S2'
_chemical_formula_weight         623.60
_chemical_name_systematic
;
Bis(acetonitrile-κN)bis(4-benzoylpyridine-κN)bis(thiocyanato-\
κN)cobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.547(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0304(6)
_cell_length_b                   8.3355(4)
_cell_length_c                   18.2581(12)
_cell_measurement_reflns_used    17991
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.69
_cell_volume                     1526.46(15)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.074
_diffrn_reflns_theta_min         2.686
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe, 2008)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.1615
_exptl_crystal_size_mid          0.0841
_exptl_crystal_size_min          0.0238
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.693
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0604P)²+0.5217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                2895
_reflns_number_total             3347
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5365sup1.cif
_cod_data_source_block           I
_cod_database_code               2242229
_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.
;
loop_
_space_group_symop_operation_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_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
Co Co1 0.5000 0.0000 0.5000 0.02109(12) Uani d 1
N N1 0.65155(15) 0.11822(18) 0.55359(9) 0.0322(3) Uani d 1
C C1 0.71187(17) 0.2142(2) 0.58531(10) 0.0313(4) Uani d 1
S S1 0.79948(6) 0.34828(9) 0.62877(5) 0.0698(3) Uani d 1
N N2 0.49639(16) -0.17253(18) 0.58858(8) 0.0311(3) Uani d 1
C C2 0.50846(19) -0.2619(2) 0.63506(10) 0.0317(4) Uani d 1
C C3 0.5267(3) -0.3769(3) 0.69412(13) 0.0514(6) Uani d 1
H H3A 0.5739 -0.4714 0.6757 0.077 Uiso calc 1
H H3B 0.4395 -0.4093 0.7128 0.077 Uiso calc 1
H H3C 0.5791 -0.3276 0.7337 0.077 Uiso calc 1
N N11 0.35979(14) 0.15671(16) 0.55624(7) 0.0234(3) Uani d 1
C C11 0.37171(18) 0.1751(2) 0.62899(9) 0.0281(4) Uani d 1
H H11 0.4386 0.1159 0.6543 0.034 Uiso calc 1
C C12 0.29053(18) 0.2770(2) 0.66876(9) 0.0283(4) Uani d 1
H H12 0.3009 0.2853 0.7204 0.034 Uiso calc 1
C C13 0.19360(17) 0.36697(18) 0.63229(9) 0.0240(3) Uani d 1
C C14 0.18049(17) 0.3477(2) 0.55676(9) 0.0266(3) Uani d 1
H H14 0.1153 0.4065 0.5299 0.032 Uiso calc 1
C C15 0.26444(17) 0.2409(2) 0.52146(9) 0.0262(3) Uani d 1
H H15 0.2538 0.2267 0.4701 0.031 Uiso calc 1
C C16 0.10657(17) 0.4749(2) 0.67758(9) 0.0253(3) Uani d 1
C C17 0.06203(16) 0.63359(18) 0.64974(9) 0.0238(3) Uani d 1
C C18 0.13193(17) 0.7173(2) 0.59627(10) 0.0296(4) Uani d 1
H H18 0.2059 0.6687 0.5729 0.036 Uiso calc 1
C C19 0.0930(2) 0.8723(2) 0.57732(12) 0.0390(4) Uani d 1
H H19 0.1417 0.9300 0.5416 0.047 Uiso calc 1
C C20 -0.0159(2) 0.9428(2) 0.61001(12) 0.0396(5) Uani d 1
H H20 -0.0419 1.0484 0.5966 0.048 Uiso calc 1
C C21 -0.08743(19) 0.8590(2) 0.66259(11) 0.0361(4) Uani d 1
H H21 -0.1631 0.9070 0.6845 0.043 Uiso calc 1
C C22 -0.04865(17) 0.7059(2) 0.68300(10) 0.0293(4) Uani d 1
H H22 -0.0968 0.6497 0.7195 0.035 Uiso calc 1
O O11 0.07747(15) 0.43077(16) 0.73898(7) 0.0373(3) Uani d 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Co1 N1 3_656 . 180.0
N1 Co1 N2 3_656 . 91.13(6)
N1 Co1 N2 . . 88.88(6)
N1 Co1 N2 3_656 3_656 88.87(6)
N1 Co1 N2 . 3_656 91.13(6)
N2 Co1 N2 . 3_656 180.0
N1 Co1 N11 3_656 3_656 88.05(6)
N1 Co1 N11 . 3_656 91.95(6)
N2 Co1 N11 . 3_656 88.24(5)
N2 Co1 N11 3_656 3_656 91.76(5)
N1 Co1 N11 3_656 . 91.95(6)
N1 Co1 N11 . . 88.05(6)
N2 Co1 N11 . . 91.76(5)
N2 Co1 N11 3_656 . 88.24(5)
N11 Co1 N11 3_656 . 180.00(5)
C1 N1 Co1 . . 162.48(14)
N1 C1 S1 . . 178.75(18)
C2 N2 Co1 . . 172.91(16)
N2 C2 C3 . . 178.8(2)
C2 C3 H3A . . 109.5
C2 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
C2 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
C15 N11 C11 . . 117.74(14)
C15 N11 Co1 . . 123.36(11)
C11 N11 Co1 . . 118.85(11)
N11 C11 C12 . . 122.79(15)
N11 C11 H11 . . 118.6
C12 C11 H11 . . 118.6
C11 C12 C13 . . 119.35(15)
C11 C12 H12 . . 120.3
C13 C12 H12 . . 120.3
C12 C13 C14 . . 118.03(15)
C12 C13 C16 . . 117.70(14)
C14 C13 C16 . . 124.24(15)
C15 C14 C13 . . 118.79(15)
C15 C14 H14 . . 120.6
C13 C14 H14 . . 120.6
N11 C15 C14 . . 123.27(15)
N11 C15 H15 . . 118.4
C14 C15 H15 . . 118.4
O11 C16 C17 . . 120.68(15)
O11 C16 C13 . . 118.05(15)
C17 C16 C13 . . 121.22(14)
C18 C17 C22 . . 119.48(16)
C18 C17 C16 . . 122.27(15)
C22 C17 C16 . . 118.06(15)
C19 C18 C17 . . 119.76(17)
C19 C18 H18 . . 120.1
C17 C18 H18 . . 120.1
C20 C19 C18 . . 120.58(19)
C20 C19 H19 . . 119.7
C18 C19 H19 . . 119.7
C19 C20 C21 . . 119.97(18)
C19 C20 H20 . . 120.0
C21 C20 H20 . . 120.0
C22 C21 C20 . . 120.19(17)
C22 C21 H21 . . 119.9
C20 C21 H21 . . 119.9
C21 C22 C17 . . 120.00(17)
C21 C22 H22 . . 120.0
C17 C22 H22 . . 120.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 N1 3_656 2.0520(15)
Co1 N1 . 2.0520(15)
Co1 N2 . 2.1647(15)
Co1 N2 3_656 2.1648(15)
Co1 N11 3_656 2.1831(13)
Co1 N11 . 2.1831(13)
N1 C1 . 1.155(2)
C1 S1 . 1.6244(18)
N2 C2 . 1.135(2)
C2 C3 . 1.453(3)
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
N11 C15 . 1.341(2)
N11 C11 . 1.341(2)
C11 C12 . 1.386(2)
C11 H11 . 0.9500
C12 C13 . 1.392(2)
C12 H12 . 0.9500
C13 C14 . 1.393(2)
C13 C16 . 1.506(2)
C14 C15 . 1.388(2)
C14 H14 . 0.9500
C15 H15 . 0.9500
C16 O11 . 1.218(2)
C16 C17 . 1.485(2)
C17 C18 . 1.394(2)
C17 C22 . 1.406(2)
C18 C19 . 1.392(3)
C18 H18 . 0.9500
C19 C20 . 1.380(3)
C19 H19 . 0.9500
C20 C21 . 1.392(3)
C20 H20 . 0.9500
C21 C22 . 1.384(3)
C21 H21 . 0.9500
C22 H22 . 0.9500
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
C3 H3A S1 1_545 0.98 2.85 3.771(3) 155.9
C11 H11 O11 2_546 0.95 2.49 3.193(2) 130.7

_cod_database_fobs_code 2242229
