#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179469 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/66/4336695.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_4336695
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         'C16 H18 Co N4 S2'
_chemical_formula_sum            'C16 H18 Co N4 S2'
_chemical_formula_weight         389.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 115.230(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.2697(6)
_cell_length_b                   39.566(3)
_cell_length_c                   9.1863(5)
_cell_measurement_reflns_used    16964
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.45
_cell_volume                     3705.4(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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16964
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.8492
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.2711
_exptl_crystal_size_mid          0.1494
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0410
_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)+(0.0621P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                6446
_reflns_number_total             8023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012235_si_004.cif
_cod_data_source_block           rm217
_cod_database_code               4336695
loop_
_symmetry_equiv_pos_as_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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.55703(6) 0.627954(16) 0.80999(7) 0.02132(13) Uani 1 1 d . . .
Co2 Co 1.06575(7) 0.622862(17) 0.83037(8) 0.02253(14) Uani 1 1 d . . .
N1 N 0.7299(4) 0.65451(10) 0.8746(5) 0.0257(9) Uani 1 1 d . . .
C1 C 0.8419(5) 0.65912(11) 0.9262(6) 0.0208(10) Uani 1 1 d . . .
S1 S 1.00121(11) 0.66519(3) 0.99984(14) 0.0303(3) Uani 1 1 d . . .
N2 N 0.8853(4) 0.59846(11) 0.7432(5) 0.0289(9) Uani 1 1 d . . .
C2 C 0.7767(5) 0.59190(12) 0.7065(6) 0.0239(11) Uani 1 1 d . . .
S2 S 0.62333(11) 0.58230(3) 0.65886(14) 0.0291(3) Uani 1 1 d . . .
N3 N 0.2433(4) 0.64813(10) 0.9163(5) 0.0300(10) Uani 1 1 d . . .
C3 C 0.3444(5) 0.65897(11) 0.9359(6) 0.0214(10) Uani 1 1 d . . .
S3 S 0.48838(11) 0.67400(3) 0.96161(14) 0.0287(3) Uani 1 1 d . . .
N4 N 0.3854(4) 0.60061(10) 0.7446(5) 0.0269(9) Uani 1 1 d . . .
C4 C 0.2798(5) 0.59128(12) 0.7118(6) 0.0230(11) Uani 1 1 d . . .
S4 S 0.12896(12) 0.57889(3) 0.66334(16) 0.0347(3) Uani 1 1 d . . .
N10 N 0.6473(4) 0.59924(9) 1.0308(5) 0.0258(9) Uani 1 1 d . . .
C10 C 0.7714(4) 0.58858(10) 1.0894(5) 0.0294(9) Uani 1 1 d . . .
H10 H 0.8242 0.5955 1.0372 0.035 Uiso 1 1 calc R . .
C11 C 0.8263(4) 0.56780(10) 1.2235(5) 0.0339(9) Uani 1 1 d . . .
H11 H 0.9154 0.5611 1.2616 0.041 Uiso 1 1 calc R . .
C12 C 0.7529(5) 0.55674(11) 1.3024(6) 0.0320(11) Uani 1 1 d . . .
C13 C 0.6241(4) 0.56873(11) 1.2428(5) 0.0350(9) Uani 1 1 d . . .
H13 H 0.5698 0.5626 1.2943 0.042 Uiso 1 1 calc R . .
C14 C 0.5756(4) 0.58948(10) 1.1088(5) 0.0322(9) Uani 1 1 d . . .
H14 H 0.4875 0.5972 1.0701 0.039 Uiso 1 1 calc R . .
C15 C 0.8045(6) 0.53185(12) 1.4396(6) 0.0384(12) Uani 1 1 d . . .
H15A H 0.8986 0.5364 1.5069 0.046 Uiso 1 1 calc R . .
H15B H 0.7569 0.5348 1.5078 0.046 Uiso 1 1 calc R . .
C16 C 0.7882(9) 0.49646(14) 1.3792(8) 0.080(2) Uani 1 1 d . . .
H16A H 0.8238 0.4808 1.4706 0.120 Uiso 1 1 calc R . .
H16B H 0.8354 0.4935 1.3118 0.120 Uiso 1 1 calc R . .
H16C H 0.6949 0.4917 1.3155 0.120 Uiso 1 1 calc R . .
N20 N 0.4647(4) 0.65676(10) 0.5894(5) 0.0266(9) Uani 1 1 d . . .
C20 C 0.3377(4) 0.66601(10) 0.5290(5) 0.0283(8) Uani 1 1 d . . .
H20 H 0.2857 0.6580 0.5805 0.034 Uiso 1 1 calc R . .
C21 C 0.2797(4) 0.68655(10) 0.3961(5) 0.0325(9) Uani 1 1 d . . .
H21 H 0.1897 0.6924 0.3582 0.039 Uiso 1 1 calc R . .
C22 C 0.3521(5) 0.69870(11) 0.3172(6) 0.0328(11) Uani 1 1 d . . .
C23 C 0.4814(5) 0.68828(11) 0.3771(5) 0.0380(10) Uani 1 1 d . . .
H23 H 0.5344 0.6953 0.3253 0.046 Uiso 1 1 calc R . .
C24 C 0.5345(4) 0.66762(10) 0.5123(5) 0.0351(9) Uani 1 1 d . . .
H24 H 0.6238 0.6610 0.5512 0.042 Uiso 1 1 calc R . .
C25 C 0.2942(6) 0.72278(12) 0.1777(7) 0.0428(13) Uani 1 1 d . . .
H25A H 0.3515 0.7236 0.1208 0.051 Uiso 1 1 calc R . .
H25B H 0.2073 0.7142 0.1012 0.051 Uiso 1 1 calc R . .
C26 C 0.2787(8) 0.75752(15) 0.2291(8) 0.072(2) Uani 1 1 d . . .
H26A H 0.2412 0.7723 0.1345 0.108 Uiso 1 1 calc R . .
H26B H 0.3646 0.7663 0.3036 0.108 Uiso 1 1 calc R . .
H26C H 0.2201 0.7569 0.2830 0.108 Uiso 1 1 calc R . .
N30 N 1.1433(4) 0.58938(10) 1.0340(5) 0.0296(9) Uani 1 1 d . . .
C30 C 1.2329(4) 0.59943(11) 1.1797(5) 0.0360(10) Uani 1 1 d . . .
H30 H 1.2614 0.6223 1.1917 0.043 Uiso 1 1 calc R . .
C31 C 1.2856(5) 0.57870(12) 1.3122(6) 0.0420(11) Uani 1 1 d . . .
H31 H 1.3498 0.5872 1.4112 0.050 Uiso 1 1 calc R . .
C32 C 1.2452(6) 0.54582(13) 1.3009(6) 0.0408(13) Uani 1 1 d . . .
C33 C 1.1508(5) 0.53501(11) 1.1510(6) 0.0457(12) Uani 1 1 d . . .
H33 H 1.1191 0.5124 1.1375 0.055 Uiso 1 1 calc R . .
C34 C 1.1036(5) 0.55723(11) 1.0225(6) 0.0397(10) Uani 1 1 d . . .
H34 H 1.0403 0.5493 0.9216 0.048 Uiso 1 1 calc R . .
C35 C 1.3021(8) 0.52160(18) 1.4429(8) 0.068(2) Uani 1 1 d . . .
H35A H 1.3426 0.5349 1.5436 0.082 Uiso 1 1 calc R . .
H35B H 1.2300 0.5080 1.4477 0.082 Uiso 1 1 calc R . .
C36 C 1.4021(9) 0.49837(18) 1.4328(9) 0.091(3) Uani 1 1 d . . .
H36A H 1.4355 0.4835 1.5270 0.136 Uiso 1 1 calc R . .
H36B H 1.4747 0.5116 1.4302 0.136 Uiso 1 1 calc R . .
H36C H 1.3621 0.4847 1.3347 0.136 Uiso 1 1 calc R . .
N40 N 0.9896(5) 0.65672(11) 0.6271(5) 0.0329(10) Uani 1 1 d . A .
C40 C 0.9034(5) 0.64712(13) 0.4802(5) 0.0467(12) Uani 1 1 d . . .
H40 H 0.8761 0.6242 0.4649 0.056 Uiso 1 1 calc R . .
C41 C 0.8523(7) 0.66841(16) 0.3509(6) 0.072(2) Uani 1 1 d . A .
H41 H 0.7920 0.6600 0.2494 0.087 Uiso 1 1 calc R . .
C42 C 0.8872(10) 0.70147(18) 0.3670(8) 0.078(2) Uani 1 1 d . . .
C43 C 0.9778(7) 0.71186(13) 0.5190(7) 0.0656(18) Uani 1 1 d . A .
H43 H 1.0060 0.7347 0.5360 0.079 Uiso 1 1 calc R . .
C44 C 1.0264(5) 0.68934(11) 0.6438(6) 0.0446(12) Uani 1 1 d . . .
H44 H 1.0884 0.6970 0.7460 0.053 Uiso 1 1 calc R A .
C45 C 0.8042(17) 0.7240(4) 0.2254(18) 0.062(4) Uiso 0.50 1 d P A 1
H45A H 0.7486 0.7396 0.2539 0.074 Uiso 0.50 1 calc PR A 1
H45B H 0.7480 0.7104 0.1304 0.074 Uiso 0.50 1 calc PR A 1
C46 C 0.9173(17) 0.7446(3) 0.1935(14) 0.082(5) Uani 0.50 1 d P A 1
H46A H 0.8754 0.7595 0.1004 0.122 Uiso 0.50 1 calc PR A 1
H46B H 0.9739 0.7284 0.1722 0.122 Uiso 0.50 1 calc PR A 1
H46C H 0.9702 0.7580 0.2887 0.122 Uiso 0.50 1 calc PR A 1
C45' C 0.8682(15) 0.7290(4) 0.2266(18) 0.067(3) Uiso 0.50 1 d P A 2
H45C H 0.9463 0.7437 0.2572 0.080 Uiso 0.50 1 calc PR A 2
H45D H 0.8498 0.7178 0.1228 0.080 Uiso 0.50 1 calc PR A 2
C46' C 0.7609(15) 0.7469(3) 0.2200(17) 0.070(4) Uani 0.50 1 d P A 2
H46D H 0.7374 0.7643 0.1363 0.104 Uiso 0.50 1 calc PR A 2
H46E H 0.7823 0.7577 0.3243 0.104 Uiso 0.50 1 calc PR A 2
H46F H 0.6867 0.7315 0.1946 0.104 Uiso 0.50 1 calc PR A 2
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'
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 N4 179.0(2) . .
N1 Co1 N10 89.36(16) . .
N4 Co1 N10 90.31(16) . .
N1 Co1 N20 91.11(16) . .
N4 Co1 N20 89.23(17) . .
N10 Co1 N20 179.3(2) . .
N1 Co1 S2 93.26(13) . .
N4 Co1 S2 85.81(13) . .
N10 Co1 S2 90.50(12) . .
N20 Co1 S2 89.93(13) . .
N1 Co1 S3 87.09(13) . .
N4 Co1 S3 93.84(13) . .
N10 Co1 S3 89.65(12) . .
N20 Co1 S3 89.92(12) . .
S2 Co1 S3 179.62(6) . .
N3 Co2 N2 178.8(2) 1_655 .
N3 Co2 N30 89.84(18) 1_655 .
N2 Co2 N30 91.00(17) . .
N3 Co2 N40 89.62(18) 1_655 .
N2 Co2 N40 89.54(18) . .
N30 Co2 N40 179.5(2) . .
N3 Co2 S1 86.11(13) 1_655 .
N2 Co2 S1 93.02(14) . .
N30 Co2 S1 89.41(13) . .
N40 Co2 S1 90.50(13) . .
N3 Co2 S4 94.84(13) 1_655 1_655
N2 Co2 S4 86.05(14) . 1_655
N30 Co2 S4 89.37(13) . 1_655
N40 Co2 S4 90.73(14) . 1_655
S1 Co2 S4 178.46(7) . 1_655
C1 N1 Co1 158.1(4) . .
N1 C1 S1 179.3(4) . .
C1 S1 Co2 101.26(17) . .
C2 N2 Co2 163.8(4) . .
N2 C2 S2 178.6(6) . .
C2 S2 Co1 102.07(18) . .
C3 N3 Co2 165.1(4) . 1_455
N3 C3 S3 179.1(5) . .
C3 S3 Co1 99.77(17) . .
C4 N4 Co1 166.7(4) . .
N4 C4 S4 178.7(5) . .
C4 S4 Co2 98.75(18) . 1_455
C10 N10 C14 117.3(4) . .
C10 N10 Co1 122.5(3) . .
C14 N10 Co1 120.1(3) . .
N10 C10 C11 122.6(4) . .
C12 C11 C10 120.9(4) . .
C11 C12 C13 116.1(4) . .
C11 C12 C15 122.8(5) . .
C13 C12 C15 121.0(5) . .
C14 C13 C12 120.0(4) . .
N10 C14 C13 123.0(4) . .
C16 C15 C12 111.1(4) . .
C24 N20 C20 117.2(4) . .
C24 N20 Co1 120.6(3) . .
C20 N20 Co1 122.1(3) . .
N20 C20 C21 123.0(4) . .
C20 C21 C22 120.3(4) . .
C23 C22 C21 116.3(4) . .
C23 C22 C25 121.9(5) . .
C21 C22 C25 121.7(5) . .
C22 C23 C24 120.7(4) . .
N20 C24 C23 122.4(4) . .
C26 C25 C22 112.5(5) . .
C34 N30 C30 116.3(4) . .
C34 N30 Co2 121.2(3) . .
C30 N30 Co2 122.5(3) . .
N30 C30 C31 124.1(4) . .
C32 C31 C30 119.8(4) . .
C31 C32 C33 117.0(4) . .
C31 C32 C35 121.9(5) . .
C33 C32 C35 121.1(5) . .
C34 C33 C32 120.0(4) . .
N30 C34 C33 122.9(4) . .
C36 C35 C32 112.9(6) . .
C40 N40 C44 116.3(4) . .
C40 N40 Co2 123.1(3) . .
C44 N40 Co2 120.5(3) . .
N40 C40 C41 123.9(5) . .
C42 C41 C40 120.3(5) . .
C41 C42 C43 116.6(5) . .
C41 C42 C45 115.3(8) . .
C43 C42 C45 127.1(8) . .
C41 C42 C45' 128.6(8) . .
C43 C42 C45' 112.9(8) . .
C45 C42 C45' 27.0(7) . .
C44 C43 C42 120.5(6) . .
N40 C44 C43 122.4(5) . .
C42 C45 C46 101.6(12) . .
C46' C45' C42 101.2(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.066(4) .
Co1 N4 2.070(4) .
Co1 N10 2.164(4) .
Co1 N20 2.166(4) .
Co1 S2 2.5754(15) .
Co1 S3 2.6032(15) .
Co2 N3 2.069(5) 1_655
Co2 N2 2.079(5) .
Co2 N30 2.150(4) .
Co2 N40 2.157(4) .
Co2 S1 2.5927(16) .
Co2 S4 2.6117(16) 1_655
N1 C1 1.157(7) .
C1 S1 1.644(6) .
N2 C2 1.152(7) .
C2 S2 1.636(6) .
N3 C3 1.158(7) .
N3 Co2 2.069(5) 1_455
C3 S3 1.648(6) .
N4 C4 1.156(7) .
C4 S4 1.638(6) .
S4 Co2 2.6117(16) 1_455
N10 C10 1.335(6) .
N10 C14 1.345(6) .
C10 C11 1.388(5) .
C11 C12 1.383(7) .
C12 C13 1.398(7) .
C12 C15 1.507(6) .
C13 C14 1.384(5) .
C15 C16 1.488(7) .
N20 C24 1.334(6) .
N20 C20 1.346(6) .
C20 C21 1.378(5) .
C21 C22 1.388(7) .
C22 C23 1.382(7) .
C22 C25 1.504(7) .
C23 C24 1.392(6) .
C25 C26 1.487(8) .
N30 C34 1.338(6) .
N30 C30 1.348(6) .
C30 C31 1.375(6) .
C31 C32 1.368(7) .
C32 C33 1.401(8) .
C32 C35 1.522(8) .
C33 C34 1.383(6) .
C35 C36 1.488(11) .
N40 C40 1.339(6) .
N40 C44 1.344(6) .
C40 C41 1.367(7) .
C41 C42 1.356(10) .
C42 C43 1.395(10) .
C42 C45 1.524(16) .
C42 C45' 1.630(17) .
C43 C44 1.369(7) .
C45 C46 1.64(2) .
C45' C46' 1.38(2) .
