#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:02:21 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179649 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/02/4510287.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_4510287
loop_
_publ_author_name
'Wöhlert, Susanne'
'Runčevski, Tomče'
'Dinnebier, Robert E.'
'Ebbinghaus, Stefan G.'
'Näther, Christian'
_publ_section_title
;
 Synthesis, Structures, Polymorphism, and Magnetic Properties of
 Transition Metal Thiocyanato Coordination Compounds
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1902
_journal_paper_doi               10.1021/cg500037d
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C30 H36 Mn N6 S2'
_chemical_formula_weight         599.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.849(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8148(3)
_cell_length_b                   16.9806(7)
_cell_length_c                   20.0807(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3297.4(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37729
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0649P)²+1.1187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                4509
_reflns_number_total             5758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Compound_1-Mn_III_RM230.CIF
_cod_data_source_block           Compound_1-Mn/III_(RM230)
_cod_original_cell_volume        3297.3(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4510287
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
Mn1 Mn 0.5000 0.5000 0.5000 0.0854(3) Uani 1 2 d S
N1 N 0.5753(3) 0.5857(2) 0.43551(17) 0.1024(9) Uani 1 1 d .
C1 C 0.5772(3) 0.6389(2) 0.40021(17) 0.0809(8) Uani 1 1 d .
S1 S 0.57992(14) 0.71395(7) 0.35106(6) 0.1147(4) Uani 1 1 d .
N10 N 0.5721(3) 0.39842(18) 0.43766(14) 0.0905(8) Uani 1 1 d .
C10 C 0.5612(5) 0.4007(3) 0.3708(2) 0.1044(11) Uani 1 1 d .
H10 H 0.5216 0.4449 0.3478 0.125 Uiso 1 1 calc R
C11 C 0.6065(5) 0.3400(3) 0.3340(2) 0.1159(14) Uani 1 1 d .
H11 H 0.5949 0.3440 0.2872 0.139 Uiso 1 1 calc R
C12 C 0.6676(5) 0.2747(3) 0.3650(2) 0.1044(12) Uani 1 1 d .
C13 C 0.6768(5) 0.2723(3) 0.4336(2) 0.1083(12) Uani 1 1 d .
H13 H 0.7162 0.2288 0.4577 0.130 Uiso 1 1 calc R
C14 C 0.6282(4) 0.3338(3) 0.4670(2) 0.1025(11) Uani 1 1 d .
H14 H 0.6351 0.3297 0.5137 0.123 Uiso 1 1 calc R
C15 C 0.7201(7) 0.2093(4) 0.3232(3) 0.153(2) Uani 1 1 d .
H15A H 0.6416 0.1780 0.3023 0.184 Uiso 1 1 calc R
H15B H 0.7598 0.2335 0.2871 0.184 Uiso 1 1 calc R
C16 C 0.8215(11) 0.1574(4) 0.3603(4) 0.216(4) Uani 1 1 d .
H16A H 0.8484 0.1187 0.3302 0.324 Uiso 1 1 calc R
H16B H 0.7827 0.1315 0.3952 0.324 Uiso 1 1 calc R
H16C H 0.9011 0.1873 0.3803 0.324 Uiso 1 1 calc R
N20 N 0.2822(3) 0.50564(17) 0.43047(14) 0.0889(8) Uani 1 1 d .
C20 C 0.1725(4) 0.4734(3) 0.4510(2) 0.1020(11) Uani 1 1 d .
H20 H 0.1863 0.4476 0.4925 0.122 Uiso 1 1 calc R
C21 C 0.0419(5) 0.4758(3) 0.4153(3) 0.1185(14) Uani 1 1 d .
H21 H -0.0301 0.4520 0.4324 0.142 Uiso 1 1 calc R
C22 C 0.0159(5) 0.5135(3) 0.3534(3) 0.1211(15) Uani 1 1 d .
C23 C 0.1281(5) 0.5444(3) 0.3314(2) 0.1186(14) Uani 1 1 d .
H23 H 0.1170 0.5692 0.2895 0.142 Uiso 1 1 calc R
C24 C 0.2567(4) 0.5397(3) 0.36997(19) 0.1034(11) Uani 1 1 d .
H24 H 0.3307 0.5615 0.3529 0.124 Uiso 1 1 calc R
C25 C -0.1320(6) 0.5217(5) 0.3128(4) 0.180(3) Uani 1 1 d .
H25A H -0.1965 0.4986 0.3388 0.215 Uiso 1 1 calc R
H25B H -0.1540 0.5773 0.3073 0.215 Uiso 1 1 calc R
C26 C -0.1518(8) 0.4868(5) 0.2496(4) 0.224(4) Uani 1 1 d .
H26A H -0.2458 0.4945 0.2278 0.336 Uiso 1 1 calc R
H26B H -0.1327 0.4315 0.2543 0.336 Uiso 1 1 calc R
H26C H -0.0905 0.5104 0.2228 0.336 Uiso 1 1 calc R
Mn2 Mn 0.5000 0.5000 0.0000 0.0876(3) Uani 1 2 d S
N2 N 0.3906(4) 0.4679(2) 0.08062(17) 0.1089(10) Uani 1 1 d .
C2 C 0.3557(4) 0.4604(2) 0.13155(18) 0.0886(9) Uani 1 1 d .
S2 S 0.3079(2) 0.45121(10) 0.20255(7) 0.1729(7) Uani 1 1 d .
N30 N 0.5945(3) 0.60860(16) 0.05884(14) 0.0904(8) Uani 1 1 d .
C30 C 0.6032(5) 0.6118(2) 0.12597(19) 0.1018(11) Uani 1 1 d .
H30 H 0.5684 0.5698 0.1476 0.122 Uiso 1 1 calc R
C31 C 0.6606(5) 0.6738(2) 0.16458(19) 0.1047(12) Uani 1 1 d .
H31 H 0.6651 0.6724 0.2112 0.126 Uiso 1 1 calc R
C32 C 0.7113(4) 0.7378(2) 0.1352(2) 0.0991(11) Uani 1 1 d .
C33 C 0.6999(5) 0.7355(2) 0.0660(2) 0.1042(12) Uani 1 1 d .
H33 H 0.7311 0.7777 0.0432 0.125 Uiso 1 1 calc R
C34 C 0.6431(4) 0.6714(2) 0.0306(2) 0.1010(11) Uani 1 1 d .
H34 H 0.6381 0.6715 -0.0161 0.121 Uiso 1 1 calc R
C35 C 0.7767(6) 0.8067(3) 0.1763(3) 0.1311(16) Uani 1 1 d .
H35A H 0.7646 0.8536 0.1484 0.157 Uiso 1 1 calc R
H35B H 0.7287 0.8150 0.2141 0.157 Uiso 1 1 calc R
C36 C 0.9204(7) 0.7964(4) 0.2016(4) 0.207(3) Uani 1 1 d .
H36A H 0.9554 0.8421 0.2270 0.310 Uiso 1 1 calc R
H36B H 0.9692 0.7893 0.1644 0.310 Uiso 1 1 calc R
H36C H 0.9333 0.7508 0.2303 0.310 Uiso 1 1 calc R
N40 N 0.6893(4) 0.42696(18) 0.05153(16) 0.0978(9) Uani 1 1 d .
C40 C 0.6783(4) 0.3633(2) 0.08815(18) 0.0972(10) Uani 1 1 d .
H40 H 0.5931 0.3526 0.1005 0.117 Uiso 1 1 calc R
C41 C 0.7848(6) 0.3121(3) 0.1090(2) 0.1106(13) Uani 1 1 d .
H41 H 0.7699 0.2681 0.1343 0.133 Uiso 1 1 calc R
C42 C 0.9125(6) 0.3250(3) 0.0930(3) 0.1193(14) Uani 1 1 d .
C43 C 0.9263(5) 0.3916(4) 0.0576(3) 0.1425(18) Uani 1 1 d .
H43 H 1.0117 0.4046 0.0466 0.171 Uiso 1 1 calc R
C44 C 0.8137(6) 0.4405(3) 0.0379(3) 0.1333(16) Uani 1 1 d .
H44 H 0.8268 0.4856 0.0136 0.160 Uiso 1 1 calc R
C45 C 1.0302(6) 0.2671(4) 0.1092(3) 0.166(2) Uani 1 1 d .
H45A H 1.1169 0.2958 0.1167 0.199 Uiso 1 1 calc R
H45B H 1.0221 0.2398 0.1507 0.199 Uiso 1 1 calc R
C46 C 1.0336(6) 0.2088(4) 0.0556(3) 0.168(2) Uani 1 1 d .
H46A H 1.1107 0.1740 0.0685 0.252 Uiso 1 1 calc R
H46B H 1.0429 0.2353 0.0144 0.252 Uiso 1 1 calc R
H46C H 0.9493 0.1789 0.0489 0.252 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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 Mn1 N1 180.00(13) . 3_666
N1 Mn1 N10 89.40(12) . 3_666
N1 Mn1 N10 90.60(12) 3_666 3_666
N1 Mn1 N10 90.60(12) . .
N1 Mn1 N10 89.40(12) 3_666 .
N10 Mn1 N10 180.000(1) 3_666 .
N1 Mn1 N20 90.80(12) . 3_666
N1 Mn1 N20 89.20(11) 3_666 3_666
N10 Mn1 N20 92.30(10) 3_666 3_666
N10 Mn1 N20 87.70(10) . 3_666
N1 Mn1 N20 89.20(11) . .
N1 Mn1 N20 90.80(12) 3_666 .
N10 Mn1 N20 87.70(10) 3_666 .
N10 Mn1 N20 92.30(10) . .
N20 Mn1 N20 180.0 3_666 .
C1 N1 Mn1 160.3(3) . .
N1 C1 S1 179.6(3) . .
C14 N10 C10 115.5(3) . .
C14 N10 Mn1 121.4(2) . .
C10 N10 Mn1 123.1(3) . .
N10 C10 C11 122.6(4) . .
C12 C11 C10 121.3(4) . .
C11 C12 C13 115.7(4) . .
C11 C12 C15 120.2(5) . .
C13 C12 C15 124.1(5) . .
C12 C13 C14 120.2(4) . .
N10 C14 C13 124.6(4) . .
C16 C15 C12 115.3(5) . .
C24 N20 C20 115.2(3) . .
C24 N20 Mn1 124.8(3) . .
C20 N20 Mn1 120.0(3) . .
N20 C20 C21 124.2(4) . .
C20 C21 C22 120.1(4) . .
C23 C22 C21 115.8(4) . .
C23 C22 C25 122.2(5) . .
C21 C22 C25 121.9(5) . .
C22 C23 C24 121.0(4) . .
N20 C24 C23 123.7(4) . .
C26 C25 C22 114.6(6) . .
N2 Mn2 N2 180.0(2) . 3_665
N2 Mn2 N30 91.47(12) . .
N2 Mn2 N30 88.53(12) 3_665 .
N2 Mn2 N30 88.53(12) . 3_665
N2 Mn2 N30 91.47(12) 3_665 3_665
N30 Mn2 N30 180.00(13) . 3_665
N2 Mn2 N40 90.35(13) . 3_665
N2 Mn2 N40 89.65(13) 3_665 3_665
N30 Mn2 N40 91.28(11) . 3_665
N30 Mn2 N40 88.72(11) 3_665 3_665
N2 Mn2 N40 89.65(13) . .
N2 Mn2 N40 90.35(13) 3_665 .
N30 Mn2 N40 88.72(11) . .
N30 Mn2 N40 91.28(11) 3_665 .
N40 Mn2 N40 180.00(13) 3_665 .
C2 N2 Mn2 164.8(4) . .
N2 C2 S2 179.2(4) . .
C34 N30 C30 115.5(3) . .
C34 N30 Mn2 124.4(2) . .
C30 N30 Mn2 120.1(3) . .
N30 C30 C31 123.4(4) . .
C32 C31 C30 120.7(4) . .
C31 C32 C33 116.0(4) . .
C31 C32 C35 122.1(4) . .
C33 C32 C35 121.9(4) . .
C34 C33 C32 120.3(4) . .
N30 C34 C33 124.0(4) . .
C36 C35 C32 113.7(4) . .
C44 N40 C40 115.1(4) . .
C44 N40 Mn2 120.9(3) . .
C40 N40 Mn2 123.3(3) . .
N40 C40 C41 124.0(4) . .
C42 C41 C40 120.7(4) . .
C43 C42 C41 115.8(4) . .
C43 C42 C45 121.0(6) . .
C41 C42 C45 123.0(5) . .
C42 C43 C44 120.3(5) . .
N40 C44 C43 124.0(5) . .
C46 C45 C42 113.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N1 2.161(3) .
Mn1 N1 2.161(3) 3_666
Mn1 N10 2.312(3) 3_666
Mn1 N10 2.312(3) .
Mn1 N20 2.346(3) 3_666
Mn1 N20 2.346(3) .
N1 C1 1.150(4) .
C1 S1 1.615(4) .
N10 C14 1.321(5) .
N10 C10 1.329(5) .
C10 C11 1.385(6) .
C11 C12 1.360(6) .
C12 C13 1.366(6) .
C12 C15 1.534(7) .
C13 C14 1.371(6) .
C15 C16 1.439(9) .
N20 C24 1.330(4) .
N20 C20 1.336(5) .
C20 C21 1.358(6) .
C21 C22 1.381(7) .
C22 C23 1.360(6) .
C22 C25 1.545(8) .
C23 C24 1.366(6) .
C25 C26 1.384(9) .
Mn2 N2 2.160(3) .
Mn2 N2 2.160(3) 3_665
Mn2 N30 2.298(3) .
Mn2 N30 2.298(3) 3_665
Mn2 N40 2.324(3) 3_665
Mn2 N40 2.324(3) .
N2 C2 1.140(4) .
C2 S2 1.583(4) .
N30 C34 1.334(5) .
N30 C30 1.337(4) .
C30 C31 1.370(5) .
C31 C32 1.370(6) .
C32 C33 1.377(6) .
C32 C35 1.509(6) .
C33 C34 1.366(5) .
C35 C36 1.425(7) .
N40 C44 1.317(6) .
N40 C40 1.323(5) .
C40 C41 1.367(6) .
C41 C42 1.364(6) .
C42 C43 1.355(7) .
C42 C45 1.510(7) .
C43 C44 1.384(7) .
C45 C46 1.465(8) .
