#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179469 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/66/4336694.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_4336694
loop_
_publ_author_name
'Susanne Wöhlert'
'Tomasz Fic'
'Zbigniew Tomkowicz'
'Stefan G. Ebbinghaus'
'Michał Rams'
'Wolfgang Haase'
'Christian Näther'
_publ_section_title
;
 Structural and Magnetic Studies of a New Co(II) Thiocyanato Coordination
 Polymer Showing Slow Magnetic Relaxations and a Metamagnetic Transition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12947
_journal_page_last               12957
_journal_paper_doi               10.1021/ic4012235
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H54 Co2 N10 S4'
_chemical_formula_sum            'C46 H54 Co2 N10 S4'
_chemical_formula_weight         993.09
_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            4
_cell_length_a                   15.5182(9)
_cell_length_b                   11.4066(4)
_cell_length_c                   27.9992(10)
_cell_measurement_reflns_used    17474
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.96
_cell_volume                     4956.1(4)
_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, 2011)
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'phi scan'
_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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17474
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.9425
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            light-red
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.1149
_exptl_crystal_size_mid          0.0725
_exptl_crystal_size_min          0.0429
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0414P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                2685
_reflns_number_total             4366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012235_si_003.cif
_cod_data_source_block           rm66
_cod_database_code               4336694
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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 0.49797(3) 0.44753(4) 0.599717(14) 0.03106(12) Uani 1 1 d .
N1 N 0.43433(19) 0.3662(3) 0.65482(10) 0.0397(7) Uani 1 1 d .
C1 C 0.4105(2) 0.3102(3) 0.68680(12) 0.0343(8) Uani 1 1 d .
S1 S 0.37703(8) 0.23095(10) 0.73138(4) 0.0538(3) Uani 1 1 d .
N2 N 0.43738(18) 0.4716(3) 0.45656(9) 0.0372(7) Uani 1 1 d .
C2 C 0.40685(19) 0.4404(3) 0.49211(10) 0.0275(7) Uani 1 1 d .
S2 S 0.36379(6) 0.39931(9) 0.54270(3) 0.0404(2) Uani 1 1 d .
N10 N 0.44417(18) 0.6163(3) 0.61874(9) 0.0358(7) Uani 1 1 d .
C10 C 0.4502(2) 0.6572(4) 0.66351(12) 0.0426(9) Uani 1 1 d .
H10 H 0.4774 0.6090 0.6867 0.051 Uiso 1 1 calc R
C11 C 0.4197(3) 0.7637(4) 0.67771(13) 0.0489(10) Uani 1 1 d .
H11 H 0.4271 0.7883 0.7098 0.059 Uiso 1 1 calc R
C12 C 0.3780(3) 0.8356(4) 0.64568(14) 0.0518(10) Uani 1 1 d .
C13 C 0.3704(3) 0.7943(3) 0.59934(14) 0.0496(10) Uani 1 1 d .
H13 H 0.3417 0.8400 0.5758 0.059 Uiso 1 1 calc R
C14 C 0.4047(2) 0.6863(3) 0.58742(12) 0.0421(9) Uani 1 1 d .
H14 H 0.3999 0.6606 0.5553 0.051 Uiso 1 1 calc R
C15 C 0.3458(5) 0.9542(5) 0.66129(18) 0.095(2) Uani 1 1 d .
H15A H 0.3147 0.9430 0.6918 0.114 Uiso 1 1 calc R
H15B H 0.3971 1.0029 0.6685 0.114 Uiso 1 1 calc R
C16 C 0.2912(4) 1.0217(5) 0.6308(2) 0.0891(19) Uani 1 1 d .
H16A H 0.2785 1.0972 0.6460 0.134 Uiso 1 1 calc R
H16B H 0.2373 0.9790 0.6253 0.134 Uiso 1 1 calc R
H16C H 0.3203 1.0352 0.6003 0.134 Uiso 1 1 calc R
N20 N 0.60989(18) 0.4781(2) 0.64378(9) 0.0335(7) Uani 1 1 d .
C20 C 0.6375(2) 0.4027(3) 0.67695(11) 0.0353(8) Uani 1 1 d .
H20 H 0.6062 0.3320 0.6815 0.042 Uiso 1 1 calc R
C21 C 0.7092(2) 0.4223(3) 0.70474(12) 0.0381(8) Uani 1 1 d .
H21 H 0.7267 0.3652 0.7274 0.046 Uiso 1 1 calc R
C22 C 0.7559(2) 0.5249(3) 0.69981(11) 0.0367(8) Uani 1 1 d .
C23 C 0.7266(2) 0.6033(3) 0.66559(12) 0.0430(9) Uani 1 1 d .
H23 H 0.7562 0.6752 0.6607 0.052 Uiso 1 1 calc R
C24 C 0.6552(2) 0.5776(3) 0.63877(12) 0.0408(9) Uani 1 1 d .
H24 H 0.6369 0.6329 0.6155 0.049 Uiso 1 1 calc R
C25 C 0.8344(2) 0.5511(4) 0.72943(13) 0.0481(10) Uani 1 1 d .
H25A H 0.8326 0.6340 0.7398 0.058 Uiso 1 1 calc R
H25B H 0.8338 0.5013 0.7584 0.058 Uiso 1 1 calc R
C26 C 0.9165(3) 0.5297(5) 0.70239(17) 0.0753(16) Uani 1 1 d .
H26A H 0.9215 0.4461 0.6948 0.113 Uiso 1 1 calc R
H26B H 0.9658 0.5538 0.7220 0.113 Uiso 1 1 calc R
H26C H 0.9159 0.5753 0.6727 0.113 Uiso 1 1 calc R
N30 N 0.54884(18) 0.2786(3) 0.57671(10) 0.0357(7) Uani 1 1 d .
C30 C 0.6262(2) 0.2666(4) 0.55617(13) 0.0450(9) Uani 1 1 d .
H30 H 0.6610 0.3345 0.5522 0.054 Uiso 1 1 calc R
C31 C 0.6578(3) 0.1605(4) 0.54053(14) 0.0506(10) Uani 1 1 d .
H31 H 0.7130 0.1572 0.5260 0.061 Uiso 1 1 calc R
C32 C 0.6107(3) 0.0593(4) 0.54562(13) 0.0461(9) Uani 1 1 d .
C33 C 0.5308(3) 0.0717(4) 0.56682(15) 0.0519(11) Uani 1 1 d .
H33 H 0.4953 0.0047 0.5714 0.062 Uiso 1 1 calc R
C34 C 0.5018(3) 0.1805(3) 0.58141(12) 0.0451(8) Uani 1 1 d .
H34 H 0.4462 0.1861 0.5954 0.054 Uiso 1 1 calc R
C35 C 0.6447(3) -0.0592(4) 0.53061(16) 0.0657(13) Uani 1 1 d .
H35A H 0.6086 -0.0895 0.5042 0.079 Uiso 1 1 calc R
H35B H 0.7041 -0.0495 0.5182 0.079 Uiso 1 1 calc R
C36 C 0.6458(4) -0.1457(5) 0.5691(2) 0.100(2) Uani 1 1 d .
H36A H 0.6678 -0.2205 0.5569 0.150 Uiso 1 1 calc R
H36B H 0.5872 -0.1567 0.5814 0.150 Uiso 1 1 calc R
H36C H 0.6832 -0.1180 0.5950 0.150 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'
Co Co 0.3494 0.9721 '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'
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 179.42(12) . 5_666
N1 Co1 N20 91.75(11) . .
N2 Co1 N20 88.47(10) 5_666 .
N1 Co1 N10 91.79(11) . .
N2 Co1 N10 88.74(11) 5_666 .
N20 Co1 N10 91.48(10) . .
N1 Co1 N30 89.83(12) . .
N2 Co1 N30 89.62(11) 5_666 .
N20 Co1 N30 91.17(11) . .
N10 Co1 N30 176.85(10) . .
N1 Co1 S2 88.92(9) . .
N2 Co1 S2 90.83(7) 5_666 .
N20 Co1 S2 176.74(8) . .
N10 Co1 S2 91.69(8) . .
N30 Co1 S2 85.64(8) . .
C1 N1 Co1 169.0(3) . .
N1 C1 S1 179.6(4) . .
C2 N2 Co1 169.4(3) . 5_666
N2 C2 S2 178.7(3) . .
C2 S2 Co1 98.03(11) . .
C14 N10 C10 116.0(3) . .
C14 N10 Co1 123.2(2) . .
C10 N10 Co1 120.8(2) . .
N10 C10 C11 123.9(4) . .
C10 C11 C12 120.3(3) . .
C11 C12 C13 116.6(4) . .
C11 C12 C15 120.1(4) . .
C13 C12 C15 123.3(4) . .
C14 C13 C12 119.7(4) . .
N10 C14 C13 123.4(3) . .
C16 C15 C12 120.5(4) . .
C20 N20 C24 116.7(3) . .
C20 N20 Co1 123.4(2) . .
C24 N20 Co1 119.9(2) . .
N20 C20 C21 123.2(3) . .
C20 C21 C22 120.3(3) . .
C21 C22 C23 116.3(3) . .
C21 C22 C25 122.5(3) . .
C23 C22 C25 121.2(3) . .
C24 C23 C22 120.4(4) . .
N20 C24 C23 123.1(3) . .
C26 C25 C22 112.2(3) . .
C30 N30 C34 116.4(3) . .
C30 N30 Co1 122.9(3) . .
C34 N30 Co1 120.7(2) . .
N30 C30 C31 123.1(4) . .
C32 C31 C30 121.1(4) . .
C31 C32 C33 115.8(4) . .
C31 C32 C35 122.5(4) . .
C33 C32 C35 121.7(4) . .
C34 C33 C32 120.7(4) . .
N30 C34 C33 122.9(4) . .
C36 C35 C32 113.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.053(3) .
Co1 N2 2.083(3) 5_666
Co1 N20 2.159(3) .
Co1 N10 2.165(3) .
Co1 N30 2.179(3) .
Co1 S2 2.6809(10) .
N1 C1 1.161(4) .
C1 S1 1.626(4) .
N2 C2 1.159(4) .
N2 Co1 2.083(3) 5_666
C2 S2 1.635(3) .
N10 C14 1.335(4) .
N10 C10 1.341(4) .
C10 C11 1.363(5) .
C11 C12 1.377(5) .
C12 C13 1.385(5) .
C12 C15 1.507(6) .
C13 C14 1.383(5) .
C15 C16 1.428(7) .
N20 C20 1.337(4) .
N20 C24 1.342(4) .
C20 C21 1.376(5) .
C21 C22 1.383(5) .
C22 C23 1.387(5) .
C22 C25 1.505(5) .
C23 C24 1.370(5) .
C25 C26 1.502(6) .
N30 C30 1.338(4) .
N30 C34 1.343(5) .
C30 C31 1.377(5) .
C31 C32 1.374(6) .
C32 C33 1.383(5) .
C32 C35 1.510(6) .
C33 C34 1.381(5) .
C35 C36 1.462(7) .
