#------------------------------------------------------------------------------
#$Date: 2019-11-16 08:08:44 +0200 (Sat, 16 Nov 2019) $
#$Revision: 227944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243201.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_2243201
loop_
_publ_author_name
'Neumann, Tristan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of pyridinium
 tetraisothiocyanatodipyridinechromium(III) pyridine monosolvate
;
_journal_coeditor_code           LH5933
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1875
_journal_page_last               1879
_journal_paper_doi               10.1107/S2056989019014488
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'(C5 H6 N) [Cr (N C S)4 (C5 H5 N1)2], C5 H5 N'
_chemical_formula_moiety
'C14 H10 Cr N6 S4 -, C5 H5.70 N +, C5 H5.30 N'
_chemical_formula_sum            'C24 H21 Cr N8 S4'
_chemical_formula_weight         601.73
_chemical_name_systematic
;
Pyridinium tetraisothiocyanatobis(pyridine)chromium(III)
pyridine monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1068(5)
_cell_length_b                   8.8168(6)
_cell_length_c                   16.2628(9)
_cell_measurement_reflns_used    12253
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.095
_cell_measurement_theta_min      2.628
_cell_volume                     1449.17(15)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 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      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe IPDS1'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12253
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.989
_diffrn_reflns_theta_min         2.628
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.7864
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.422
_refine_ls_abs_structure_details
;
Flack x determined using 925 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.027(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0428
_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)+(0.0503P)²+0.4808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                2452
_reflns_number_total             3153
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lh5933sup1.cif
_cod_data_source_block           I
_cod_database_code               2243201
_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, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
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
Cr Cr1 0.500000 0.64497(13) 0.99944(7) 0.0350(3) Uani d 1
N N1 0.6380(5) 0.5526(5) 0.9278(3) 0.0456(11) Uani d 1
C C1 0.7030(6) 0.4870(6) 0.8803(3) 0.0409(12) Uani d 1
S S1 0.7901(2) 0.39515(18) 0.81396(11) 0.0671(5) Uani d 1
N N2 0.3635(5) 0.7405(5) 1.0697(3) 0.0453(11) Uani d 1
C C2 0.2924(6) 0.8219(6) 1.1063(3) 0.0410(12) Uani d 1
S S2 0.1955(2) 0.9312(2) 1.15735(11) 0.0689(5) Uani d 1
N N11 0.500000 0.8403(7) 0.9254(4) 0.0378(13) Uani d 1
C C11 0.6137(6) 0.9059(6) 0.9028(3) 0.0446(13) Uani d 1
H H11 0.693081 0.859637 0.917262 0.053 Uiso calc 1
C C12 0.6175(7) 1.0412(6) 0.8584(4) 0.0522(14) Uani d 1
H H12 0.697858 1.084674 0.843515 0.063 Uiso calc 1
C C13 0.500000 1.1087(10) 0.8372(5) 0.054(2) Uani d 1
H H13 0.499999 1.200033 0.808600 0.065 Uiso calc 1
N N21 0.500000 0.4529(7) 1.0738(4) 0.0380(14) Uani d 1
C C21 0.500000 0.4633(10) 1.1565(5) 0.051(2) Uani d 1
H H21 0.500000 0.558953 1.180637 0.061 Uiso calc 1
C C22 0.500000 0.3371(11) 1.2067(6) 0.065(3) Uani d 1
H H22 0.500000 0.348073 1.263584 0.078 Uiso calc 1
C C23 0.500000 0.1953(12) 1.1719(6) 0.068(3) Uani d 1
H H23 0.500000 0.109435 1.205088 0.082 Uiso calc 1
C C24 0.500000 0.1805(10) 1.0868(6) 0.059(2) Uani d 1
H H24 0.500000 0.085445 1.061946 0.070 Uiso calc 1
C C25 0.500000 0.3110(9) 1.0405(5) 0.0441(18) Uani d 1
H H25 0.500000 0.301981 0.983543 0.053 Uiso calc 1
N N31 0.000000 1.0017(9) 0.4322(5) 0.061(2) Uani d 1
H H31A 0.000000 0.920955 0.461881 0.073 Uiso calc 0.3
C C31 0.000000 0.9933(10) 0.3502(6) 0.057(2) Uani d 1
H H31 0.000000 0.898380 0.325264 0.068 Uiso calc 1
C C32 0.000000 1.1428(12) 0.4678(6) 0.062(2) Uani d 1
H H32 0.000000 1.150849 0.524812 0.075 Uiso calc 1
C C33 0.000000 1.2701(11) 0.4217(6) 0.060(2) Uani d 1
H H33 0.000000 1.364655 0.447130 0.072 Uiso calc 1
C C34 0.000000 1.2604(10) 0.3374(5) 0.051(2) Uani d 1
H H34 0.000000 1.347438 0.305068 0.061 Uiso calc 1
C C35 0.000000 1.1195(10) 0.3021(5) 0.051(2) Uani d 1
H H35 0.000000 1.109984 0.245176 0.062 Uiso calc 1
N N41 0.000000 0.7526(8) 0.5271(5) 0.0557(19) Uani d 1
H H41A 0.000000 0.832178 0.496530 0.067 Uiso calc 0.7
C C41 0.1138(8) 0.6919(8) 0.5505(5) 0.0686(19) Uani d 1
H H41 0.192859 0.735531 0.533295 0.082 Uiso calc 1
C C42 0.1165(8) 0.5636(8) 0.6004(5) 0.071(2) Uani d 1
H H42 0.196943 0.522486 0.617040 0.085 Uiso calc 1
C C43 0.000000 0.4985(10) 0.6248(5) 0.057(2) Uani d 1
H H43 0.000001 0.411685 0.657268 0.069 Uiso calc 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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 Cr1 N2 4_655 . 88.4(3) y
N2 Cr1 N1 4_655 . 91.33(18) y
N2 Cr1 N1 . . 178.9(2) y
N2 Cr1 N1 4_655 4_655 178.9(2) y
N2 Cr1 N1 . 4_655 91.33(18) y
N1 Cr1 N1 . 4_655 88.9(3) y
N2 Cr1 N21 4_655 . 90.62(18) y
N2 Cr1 N21 . . 90.62(18) y
N1 Cr1 N21 . . 90.39(18) y
N1 Cr1 N21 4_655 . 90.40(18) y
N2 Cr1 N11 4_655 . 88.98(18) y
N2 Cr1 N11 . . 88.98(18) y
N1 Cr1 N11 . . 90.00(18) y
N1 Cr1 N11 4_655 . 90.00(18) y
N21 Cr1 N11 . . 179.4(3) y
C1 N1 Cr1 . . 169.7(5) ?
N1 C1 S1 . . 178.9(6) ?
C2 N2 Cr1 . . 167.6(5) ?
N2 C2 S2 . . 179.1(5) ?
C11 N11 C11 . 4_655 118.4(7) ?
C11 N11 Cr1 . . 120.8(3) ?
C11 N11 Cr1 4_655 . 120.7(3) ?
N11 C11 C12 . . 122.4(6) ?
N11 C11 H11 . . 118.8 ?
C12 C11 H11 . . 118.8 ?
C13 C12 C11 . . 118.5(6) ?
C13 C12 H12 . . 120.8 ?
C11 C12 H12 . . 120.8 ?
C12 C13 C12 4_655 . 119.8(8) ?
C12 C13 H13 4_655 . 120.1 ?
C12 C13 H13 . . 120.1 ?
C21 N21 C25 . . 117.3(7) ?
C21 N21 Cr1 . . 121.6(5) ?
C25 N21 Cr1 . . 121.1(5) ?
N21 C21 C22 . . 122.4(8) ?
N21 C21 H21 . . 118.8 ?
C22 C21 H21 . . 118.8 ?
C23 C22 C21 . . 119.4(8) ?
C23 C22 H22 . . 120.3 ?
C21 C22 H22 . . 120.3 ?
C22 C23 C24 . . 119.8(9) ?
C22 C23 H23 . . 120.1 ?
C24 C23 H23 . . 120.1 ?
C25 C24 C23 . . 117.8(9) ?
C25 C24 H24 . . 121.1 ?
C23 C24 H24 . . 121.1 ?
N21 C25 C24 . . 123.5(7) ?
N21 C25 H25 . . 118.3 ?
C24 C25 H25 . . 118.3 ?
C31 N31 C32 . . 118.1(8) ?
C31 N31 H31A . . 120.9 ?
C32 N31 H31A . . 120.9 ?
N31 C31 C35 . . 121.9(8) ?
N31 C31 H31 . . 119.0 ?
C35 C31 H31 . . 119.0 ?
C33 C32 N31 . . 121.4(9) ?
C33 C32 H32 . . 119.3 ?
N31 C32 H32 . . 119.3 ?
C32 C33 C34 . . 120.1(9) ?
C32 C33 H33 . . 119.9 ?
C34 C33 H33 . . 119.9 ?
C35 C34 C33 . . 118.3(8) ?
C35 C34 H34 . . 120.8 ?
C33 C34 H34 . . 120.8 ?
C31 C35 C34 . . 120.1(8) ?
C31 C35 H35 . . 119.9 ?
C34 C35 H35 . . 119.9 ?
C41 N41 C41 . 4 120.6(8) ?
C41 N41 H41A . . 119.7 ?
C41 N41 H41A 4 . 119.7 ?
N41 C41 C42 . . 120.9(7) ?
N41 C41 H41 . . 119.6 ?
C42 C41 H41 . . 119.6 ?
C43 C42 C41 . . 119.5(7) ?
C43 C42 H42 . . 120.3 ?
C41 C42 H42 . . 120.3 ?
C42 C43 C42 . 4 118.7(8) ?
C42 C43 H43 . . 120.6 ?
C42 C43 H43 4 . 120.6 ?
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
Cr1 N2 4_655 1.980(5) y
Cr1 N2 . 1.980(5) y
Cr1 N1 . 1.991(5) y
Cr1 N1 4_655 1.991(5) y
Cr1 N21 . 2.080(6) y
Cr1 N11 . 2.102(6) y
N1 C1 . 1.168(7) ?
C1 S1 . 1.610(6) ?
N2 C2 . 1.177(7) ?
C2 S2 . 1.605(6) ?
N11 C11 . 1.338(7) ?
N11 C11 4_655 1.338(7) ?
C11 C12 . 1.395(7) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.373(8) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
N21 C21 . 1.349(10) ?
N21 C25 . 1.363(10) ?
C21 C22 . 1.379(12) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.373(15) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.390(13) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.375(11) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
N31 C31 . 1.336(13) ?
N31 C32 . 1.372(13) ?
N31 H31A . 0.8600 ?
C31 C35 . 1.360(13) ?
C31 H31 . 0.9300 ?
C32 C33 . 1.350(13) ?
C32 H32 . 0.9300 ?
C33 C34 . 1.375(12) ?
C33 H33 . 0.9300 ?
C34 C35 . 1.368(11) ?
C34 H34 . 0.9300 ?
C35 H35 . 0.9300 ?
N41 C41 . 1.324(8) ?
N41 C41 4 1.324(8) ?
N41 H41A . 0.8600 ?
C41 C42 . 1.393(9) ?
C41 H41 . 0.9300 ?
C42 C43 . 1.369(9) ?
C42 H42 . 0.9300 ?
C43 H43 . 0.9300 ?
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
_geom_hbond_publ_flag
C12 H12 S1 1_565 0.93 2.93 3.647(6) 134.8 yes
C32 H32 S2 2_574 0.93 3.01 3.719(8) 134.0 yes
C32 H32 S2 3_574 0.93 3.01 3.719(8) 134.0 yes
C35 H35 S2 1_554 0.93 2.90 3.494(7) 122.6 yes
C35 H35 S2 4_554 0.93 2.90 3.494(7) 122.6 yes
N31 H31A N41 . 0.86 1.82 2.684(11) 178.6 yes
N41 H41A N31 . 0.86 1.82 2.684(11) 179.6 yes

_cod_database_fobs_code 2243201
