#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:16:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179529 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/26/4342641.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4342641
loop_
_publ_author_name
'Werner, Julia'
'Rams, Michał'
'Tomkowicz, Zbigniew'
'Runčevski, Tomče'
'Dinnebier, Robert E.'
'Suckert, Stefan'
'Näther, Christian'
_publ_section_title
;
 Thermodynamically metastable thiocyanato coordination polymer that shows
 slow relaxations of the magnetization.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2893
_journal_page_last               2901
_journal_paper_doi               10.1021/ic503029t
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C16 H14 Co N4 O2 S2'
_chemical_formula_sum            'C16 H14 Co N4 O2 S2'
_chemical_formula_weight         417.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.5315(3)
_cell_length_b                   15.8242(4)
_cell_length_c                   24.3712(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3675.87(17)
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_collection       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32860
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.8194
_exptl_absorpt_correction_T_min  0.7238
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red 32 (STOE, 2008)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0274P)²+2.1153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3747
_reflns_number_total             4408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503029t_si_003.cif
_cod_data_source_block           jw361
_cod_depositor_comments
'Adding full bibliography for 4342640--4342641.cif.'
_cod_database_code               4342641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.68668(3) 0.63951(2) 0.493970(15) 0.04041(11) Uani 1 1 d .
N1 N 0.5128(2) 0.40272(15) 0.52419(10) 0.0458(5) Uani 1 1 d .
C1 C 0.6092(3) 0.44287(17) 0.53539(11) 0.0387(5) Uani 1 1 d .
S1 S 0.74461(8) 0.50175(5) 0.55127(4) 0.05259(19) Uani 1 1 d .
N2 N 0.8894(2) 0.67246(16) 0.51474(11) 0.0494(6) Uani 1 1 d .
C2 C 0.9957(3) 0.69287(17) 0.53263(12) 0.0424(6) Uani 1 1 d .
S2 S 1.14921(8) 0.72054(5) 0.55763(4) 0.0543(2) Uani 1 1 d .
N11 N 0.7553(2) 0.57843(15) 0.41871(10) 0.0459(5) Uani 1 1 d .
O11 O 0.9638(4) 0.3961(3) 0.27354(14) 0.1152(13) Uani 1 1 d .
C11 C 0.6766(3) 0.5832(2) 0.37343(13) 0.0540(7) Uani 1 1 d .
H11 H 0.5958 0.6161 0.3745 0.065 Uiso 1 1 calc R
C12 C 0.7083(3) 0.5422(2) 0.32539(13) 0.0536(7) Uani 1 1 d .
H12 H 0.6506 0.5480 0.2948 0.064 Uiso 1 1 calc R
C13 C 0.8271(3) 0.4923(2) 0.32302(13) 0.0514(7) Uani 1 1 d .
C14 C 0.9086(3) 0.4863(2) 0.36965(14) 0.0568(8) Uani 1 1 d .
H14 H 0.9887 0.4528 0.3697 0.068 Uiso 1 1 calc R
C15 C 0.8704(3) 0.5302(2) 0.41600(13) 0.0527(7) Uani 1 1 d .
H15 H 0.9273 0.5262 0.4469 0.063 Uiso 1 1 calc R
C16 C 0.8712(4) 0.4476(3) 0.27107(16) 0.0677(9) Uani 1 1 d .
C17 C 0.8036(5) 0.4702(3) 0.21806(16) 0.0841(12) Uani 1 1 d .
H17A H 0.8377 0.4335 0.1897 0.126 Uiso 1 1 calc R
H17B H 0.8256 0.5277 0.2089 0.126 Uiso 1 1 calc R
H17C H 0.7037 0.4639 0.2213 0.126 Uiso 1 1 calc R
N21 N 0.6060(2) 0.69526(15) 0.56784(10) 0.0445(5) Uani 1 1 d .
O21 O 0.5106(3) 0.8686(2) 0.73389(11) 0.0830(8) Uani 1 1 d .
C21 C 0.5023(3) 0.6589(2) 0.59622(13) 0.0513(7) Uani 1 1 d .
H21 H 0.4651 0.6084 0.5832 0.062 Uiso 1 1 calc R
C22 C 0.4482(3) 0.6923(2) 0.64354(13) 0.0551(8) Uani 1 1 d .
H22 H 0.3760 0.6646 0.6619 0.066 Uiso 1 1 calc R
C23 C 0.5013(3) 0.7673(2) 0.66389(12) 0.0493(7) Uani 1 1 d .
C24 C 0.6070(3) 0.8065(2) 0.63377(13) 0.0542(7) Uani 1 1 d .
H24 H 0.6442 0.8577 0.6455 0.065 Uiso 1 1 calc R
C25 C 0.6562(3) 0.76902(19) 0.58679(13) 0.0516(7) Uani 1 1 d .
H25 H 0.7272 0.7958 0.5672 0.062 Uiso 1 1 calc R
C26 C 0.4519(4) 0.8060(3) 0.71648(14) 0.0626(9) Uani 1 1 d .
C27 C 0.3304(5) 0.7673(3) 0.74566(19) 0.0906(14) Uani 1 1 d .
H27A H 0.3568 0.7127 0.7594 0.136 Uiso 1 1 calc R
H27B H 0.2532 0.7613 0.7207 0.136 Uiso 1 1 calc R
H27C H 0.3031 0.8029 0.7757 0.136 Uiso 1 1 calc R
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_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Co1 N2 175.48(10) 5_666 .
N1 Co1 N21 89.02(9) 5_666 .
N2 Co1 N21 91.48(10) . .
N1 Co1 N11 87.27(10) 5_666 .
N2 Co1 N11 92.15(10) . .
N21 Co1 N11 176.18(9) . .
N1 Co1 S2 92.63(7) 5_666 4_466
N2 Co1 S2 91.86(8) . 4_466
N21 Co1 S2 90.37(7) . 4_466
N11 Co1 S2 90.69(7) . 4_466
N1 Co1 S1 92.22(7) 5_666 .
N2 Co1 S1 83.30(7) . .
N21 Co1 S1 88.32(7) . .
N11 Co1 S1 90.93(7) . .
S2 Co1 S1 174.95(3) 4_466 .
C1 N1 Co1 165.0(2) . 5_666
N1 C1 S1 178.9(3) . .
C1 S1 Co1 100.34(9) . .
C2 N2 Co1 171.5(3) . .
N2 C2 S2 178.9(3) . .
C2 S2 Co1 99.89(10) . 4_566
C11 N11 C15 116.9(3) . .
C11 N11 Co1 120.15(19) . .
C15 N11 Co1 122.8(2) . .
N11 C11 C12 123.6(3) . .
C11 C12 C13 119.1(3) . .
C14 C13 C12 117.8(3) . .
C14 C13 C16 120.1(3) . .
C12 C13 C16 122.1(3) . .
C15 C14 C13 119.5(3) . .
N11 C15 C14 123.1(3) . .
O11 C16 C17 121.6(4) . .
O11 C16 C13 118.7(4) . .
C17 C16 C13 119.7(3) . .
C21 N21 C25 117.4(3) . .
C21 N21 Co1 121.4(2) . .
C25 N21 Co1 121.2(2) . .
N21 C21 C22 123.2(3) . .
C21 C22 C23 119.7(3) . .
C22 C23 C24 117.2(3) . .
C22 C23 C26 122.9(3) . .
C24 C23 C26 119.8(3) . .
C25 C24 C23 119.7(3) . .
N21 C25 C24 122.7(3) . .
O21 C26 C27 121.8(4) . .
O21 C26 C23 119.2(3) . .
C27 C26 C23 119.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.064(2) 5_666
Co1 N2 2.065(2) .
Co1 N21 2.147(2) .
Co1 N11 2.174(2) .
Co1 S2 2.5717(9) 4_466
Co1 S1 2.6472(9) .
N1 C1 1.150(3) .
N1 Co1 2.064(2) 5_666
C1 S1 1.638(3) .
N2 C2 1.149(3) .
C2 S2 1.644(3) .
S2 Co1 2.5717(9) 4_566
N11 C11 1.337(4) .
N11 C15 1.338(4) .
O11 C16 1.202(5) .
C11 C12 1.372(4) .
C12 C13 1.382(4) .
C13 C14 1.380(4) .
C13 C16 1.510(5) .
C14 C15 1.375(4) .
C16 C17 1.487(5) .
N21 C21 1.337(4) .
N21 C25 1.343(4) .
O21 C26 1.213(5) .
C21 C22 1.369(4) .
C22 C23 1.383(4) .
C23 C24 1.392(4) .
C23 C26 1.496(5) .
C24 C25 1.372(4) .
C26 C27 1.491(6) .
