#------------------------------------------------------------------------------
#$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $
#$Revision: 88064 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/30/2013000.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_2013000
loop_
_publ_author_name
'Kim, Jinkwon'
'Han, Sujin'
_publ_section_title
<i>trans</i>-Bis(isothiocyanato-\k<i>N</i>)bis(methanol-\k<i>O</i>)bis[2,4,6-tri(4-pyridyl)-1,3,5-triazine-\k<i>N</i>^2^]manganese(II)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m521
_journal_page_last               m522
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mn (NCS)2 (C18 H12 N6)2 (CH4 O)2]'
_chemical_formula_moiety         'C40 H32 Mn N14 O2 S2'
_chemical_formula_sum            'C40 H32 Mn N14 O2 S2'
_chemical_formula_weight         859.86
_chemical_name_systematic
;
trans-Bis(isothiocyanato-\kN)bis(methanol-\kO)bis[2,4,6-tri(4-pyridyl)-
1,3,5-triazine-\kN^4^]manganese(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.54(2)
_cell_angle_beta                 100.60(2)
_cell_angle_gamma                100.93(3)
_cell_formula_units_Z            1
_cell_length_a                   8.871(2)
_cell_length_b                   8.875(2)
_cell_length_c                   14.161(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      23
_cell_volume                     1015.3(5)
_computing_cell_refinement       'CELDIM (Enraf-Nonius, 1996)'
_computing_data_collection       'MACH3 (Enraf-Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.015
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3732
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             443
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^+1.8244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.122
_refine_ls_wR_factor_ref         0.132
_reflns_number_gt                2796
_reflns_number_total             3571
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    ob1080.cif
_[local]_cod_data_source_block   I
_cod_original_cell_volume        1015.3(4)
_cod_database_code               2013000
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mn 0.0000 0.5000 0.5000 0.0432(2) Uani d S 1 . . Mn
S1 0.47224(15) 0.94996(17) 0.64967(12) 0.1000(5) Uani d . 1 . . S
O1 0.1548(3) 0.3334(3) 0.50854(18) 0.0533(6) Uani d . 1 . . O
N1 0.0756(3) 0.5107(3) 0.3506(2) 0.0449(7) Uani d . 1 . . N
N2 -0.0462(4) -0.0343(4) -0.3631(2) 0.0521(8) Uani d . 1 . . N
N3 0.7438(4) 0.9846(4) -0.0133(3) 0.0675(10) Uani d . 1 . . N
N4 0.1260(3) 0.3744(3) -0.00988(19) 0.0387(6) Uani d . 1 . . N
N5 0.2930(3) 0.4871(3) -0.0984(2) 0.0394(6) Uani d . 1 . . N
N6 0.3276(3) 0.6188(3) 0.0776(2) 0.0393(6) Uani d . 1 . . N
N7 0.1939(4) 0.7064(4) 0.5872(2) 0.0578(9) Uani d . 1 . . N
C1 0.2076(4) 0.4987(4) 0.0733(2) 0.0363(7) Uani d . 1 . . C
C2 0.1639(4) 0.5025(4) 0.1700(2) 0.0370(7) Uani d . 1 . . C
C3 0.2435(4) 0.6251(4) 0.2606(2) 0.0469(9) Uani d . 1 . . C
H3 0.3276 0.7073 0.2624 0.056 Uiso calc R 1 . . H
C4 0.1969(4) 0.6243(4) 0.3480(3) 0.0502(9) Uani d . 1 . . C
H4 0.2526 0.7069 0.4085 0.060 Uiso calc R 1 . . H
C5 0.0011(4) 0.3934(4) 0.2626(3) 0.0478(9) Uani d . 1 . . C
H5 -0.0825 0.3125 0.2628 0.057 Uiso calc R 1 . . H
C6 0.0389(4) 0.3835(4) 0.1717(2) 0.0447(8) Uani d . 1 . . C
H6 -0.0180 0.2987 0.1125 0.054 Uiso calc R 1 . . H
C7 0.1752(4) 0.3728(4) -0.0934(2) 0.0367(7) Uani d . 1 . . C
C8 0.0955(4) 0.2325(4) -0.1874(2) 0.0372(7) Uani d . 1 . . C
C9 -0.0346(4) 0.1154(4) -0.1909(3) 0.0475(9) Uani d . 1 . . C
H9 -0.0767 0.1241 -0.1347 0.057 Uiso calc R 1 . . H
C10 -0.1004(5) -0.0139(5) -0.2793(3) 0.0555(10) Uani d . 1 . . C
H10 -0.1879 -0.0922 -0.2811 0.067 Uiso calc R 1 . . H
C11 0.0791(5) 0.0787(4) -0.3582(3) 0.0535(10) Uani d . 1 . . C
H11 0.1203 0.0662 -0.4149 0.064 Uiso calc R 1 . . H
C12 0.1514(4) 0.2139(4) -0.2733(3) 0.0497(9) Uani d . 1 . . C
H12 0.2371 0.2919 -0.2741 0.060 Uiso calc R 1 . . H
C13 0.3636(4) 0.6082(4) -0.0108(2) 0.0360(7) Uani d . 1 . . C
C14 0.4958(4) 0.7385(4) -0.0122(3) 0.0406(8) Uani d . 1 . . C
C15 0.5396(5) 0.7360(5) -0.1013(3) 0.0547(10) Uani d . 1 . . C
H15 0.4874 0.6531 -0.1623 0.066 Uiso calc R 1 . . H
C16 0.6650(5) 0.8621(6) -0.0966(4) 0.0684(12) Uani d . 1 . . C
H16 0.6950 0.8596 -0.1565 0.082 Uiso calc R 1 . . H
C17 0.6980(5) 0.9843(5) 0.0704(4) 0.0600(11) Uani d . 1 . . C
H17 0.7511 1.0698 0.1300 0.072 Uiso calc R 1 . . H
C18 0.5770(4) 0.8658(4) 0.0755(3) 0.0465(8) Uani d . 1 . . C
H18 0.5508 0.8718 0.1369 0.056 Uiso calc R 1 . . H
C19 0.3104(4) 0.8081(4) 0.6145(3) 0.0489(9) Uani d . 1 . . C
C20 0.3237(5) 0.3697(6) 0.5338(4) 0.0860(15) Uani d . 1 . . C
H20A 0.3565 0.2719 0.5312 0.129 Uiso calc R 1 . . H
H20B 0.3655 0.4472 0.6012 0.129 Uiso calc R 1 . . H
H20C 0.3627 0.4144 0.4861 0.129 Uiso calc R 1 . . H
HO1 0.1106 0.2263 0.4600 0.070 Uiso d . 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mn 0.0467(4) 0.0380(4) 0.0323(4) -0.0092(3) 0.0170(3) 0.0012(3)
S1 0.0584(7) 0.0829(9) 0.1141(11) -0.0299(7) 0.0238(7) -0.0047(8)
O1 0.0539(15) 0.0430(14) 0.0493(14) -0.0024(11) 0.0150(12) 0.0031(11)
N1 0.0499(17) 0.0417(15) 0.0356(15) -0.0031(13) 0.0169(13) 0.0070(12)
N2 0.062(2) 0.0448(17) 0.0392(16) 0.0033(15) 0.0156(14) 0.0031(13)
N3 0.056(2) 0.056(2) 0.100(3) 0.0045(17) 0.031(2) 0.038(2)
N4 0.0396(15) 0.0407(15) 0.0323(14) 0.0026(12) 0.0143(12) 0.0086(12)
N5 0.0392(15) 0.0401(15) 0.0392(15) 0.0049(12) 0.0163(12) 0.0132(12)
N6 0.0403(15) 0.0364(14) 0.0381(15) 0.0009(12) 0.0159(12) 0.0100(12)
N7 0.061(2) 0.0466(18) 0.0457(18) -0.0127(16) 0.0201(15) -0.0017(14)
C1 0.0357(17) 0.0384(17) 0.0350(17) 0.0079(14) 0.0130(13) 0.0109(14)
C2 0.0389(17) 0.0358(17) 0.0355(17) 0.0048(14) 0.0166(14) 0.0092(13)
C3 0.047(2) 0.0432(19) 0.0399(19) -0.0082(15) 0.0160(15) 0.0076(15)
C4 0.056(2) 0.047(2) 0.0348(18) -0.0079(17) 0.0161(16) 0.0051(15)
C5 0.050(2) 0.0443(19) 0.0388(18) -0.0087(16) 0.0218(16) 0.0056(15)
C6 0.049(2) 0.0403(18) 0.0334(17) -0.0049(15) 0.0136(15) 0.0040(14)
C7 0.0347(16) 0.0369(17) 0.0377(17) 0.0066(13) 0.0140(14) 0.0096(14)
C8 0.0407(18) 0.0374(17) 0.0310(16) 0.0057(14) 0.0094(14) 0.0099(13)
C9 0.047(2) 0.048(2) 0.0419(19) 0.0020(16) 0.0203(16) 0.0064(16)
C10 0.050(2) 0.051(2) 0.051(2) -0.0069(17) 0.0184(17) 0.0037(17)
C11 0.065(2) 0.054(2) 0.0323(18) -0.0005(19) 0.0197(17) 0.0068(16)
C12 0.055(2) 0.047(2) 0.0406(19) -0.0025(17) 0.0181(16) 0.0112(16)
C13 0.0351(16) 0.0377(17) 0.0367(17) 0.0070(13) 0.0134(13) 0.0136(14)
C14 0.0388(18) 0.0378(17) 0.051(2) 0.0079(14) 0.0188(15) 0.0195(15)
C15 0.060(2) 0.050(2) 0.059(2) 0.0075(18) 0.0312(19) 0.0209(18)
C16 0.074(3) 0.069(3) 0.084(3) 0.016(2) 0.049(3) 0.041(3)
C17 0.048(2) 0.043(2) 0.081(3) -0.0017(17) 0.009(2) 0.023(2)
C18 0.0418(19) 0.0435(19) 0.053(2) 0.0026(15) 0.0125(16) 0.0187(16)
C19 0.051(2) 0.048(2) 0.0358(18) -0.0002(18) 0.0157(16) 0.0008(15)
C20 0.057(3) 0.072(3) 0.109(4) -0.002(2) 0.018(3) 0.013(3)
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
Mn N7 . 2.139(3) yes
Mn N7 2_566 2.139(3) ?
Mn O1 2_566 2.213(3) ?
Mn O1 . 2.213(3) yes
Mn N1 2_566 2.355(3) ?
Mn N1 . 2.355(3) yes
S1 C19 . 1.609(4) yes
O1 C20 . 1.425(5) yes
O1 HO1 . 0.9578 ?
N1 C5 . 1.331(4) ?
N1 C4 . 1.342(4) ?
N2 C11 . 1.325(5) ?
N2 C10 . 1.338(5) ?
N3 C16 . 1.320(6) ?
N3 C17 . 1.321(5) ?
N4 C1 . 1.331(4) ?
N4 C7 . 1.332(4) ?
N5 C13 . 1.337(4) ?
N5 C7 . 1.339(4) ?
N6 C13 . 1.330(4) ?
N6 C1 . 1.335(4) ?
N7 C19 . 1.155(4) yes
C1 C2 . 1.484(4) ?
C2 C3 . 1.381(4) ?
C2 C6 . 1.388(4) ?
C3 C4 . 1.377(5) ?
C3 H3 . 0.9300 ?
C4 H4 . 0.9300 ?
C5 C6 . 1.372(4) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.482(4) ?
C8 C12 . 1.375(5) ?
C8 C9 . 1.382(4) ?
C9 C10 . 1.373(5) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.378(5) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.490(4) ?
C14 C18 . 1.379(5) ?
C14 C15 . 1.383(5) ?
C15 C16 . 1.398(5) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
C17 C18 . 1.381(5) ?
C17 H17 . 0.9300 ?
C18 H18 . 0.9300 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9600 ?
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N7 Mn N7 . 2_566 180.0 ?
N7 Mn O1 . 2_566 88.97(12) ?
N7 Mn O1 2_566 2_566 91.03(12) ?
N7 Mn O1 . . 91.03(12) yes
N7 Mn O1 2_566 . 88.97(12) ?
O1 Mn O1 2_566 . 180.0000(10) ?
N7 Mn N1 . 2_566 90.43(11) ?
N7 Mn N1 2_566 2_566 89.57(11) ?
O1 Mn N1 2_566 2_566 86.55(10) ?
O1 Mn N1 . 2_566 93.45(10) ?
N7 Mn N1 . . 89.57(11) yes
N7 Mn N1 2_566 . 90.43(11) ?
O1 Mn N1 2_566 . 93.45(10) ?
O1 Mn N1 . . 86.55(10) yes
N1 Mn N1 2_566 . 180.0000(10) ?
C20 O1 Mn . . 128.8(3) yes
C20 O1 HO1 . . 110.2 ?
Mn O1 HO1 . . 113.6 ?
C5 N1 C4 . . 116.1(3) ?
C5 N1 Mn . . 119.5(2) ?
C4 N1 Mn . . 124.3(2) ?
C11 N2 C10 . . 116.6(3) ?
C16 N3 C17 . . 116.0(3) ?
C1 N4 C7 . . 114.8(3) ?
C13 N5 C7 . . 115.0(3) ?
C13 N6 C1 . . 114.6(3) ?
C19 N7 Mn . . 164.5(3) yes
N4 C1 N6 . . 125.6(3) ?
N4 C1 C2 . . 117.3(3) ?
N6 C1 C2 . . 117.0(3) ?
C3 C2 C6 . . 117.8(3) ?
C3 C2 C1 . . 121.6(3) ?
C6 C2 C1 . . 120.6(3) ?
C2 C3 C4 . . 119.3(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
N1 C4 C3 . . 123.5(3) ?
N1 C4 H4 . . 118.2 ?
C3 C4 H4 . . 118.3 ?
N1 C5 C6 . . 124.6(3) ?
N1 C5 H5 . . 117.7 ?
C6 C5 H5 . . 117.7 ?
C5 C6 C2 . . 118.6(3) ?
C5 C6 H6 . . 120.7 ?
C2 C6 H6 . . 120.7 ?
N4 C7 N5 . . 124.9(3) ?
N4 C7 C8 . . 117.5(3) ?
N5 C7 C8 . . 117.6(3) ?
C12 C8 C9 . . 118.1(3) ?
C12 C8 C7 . . 120.6(3) ?
C9 C8 C7 . . 121.3(3) ?
C10 C9 C8 . . 118.5(3) ?
C10 C9 H9 . . 120.8 ?
C8 C9 H9 . . 120.8 ?
N2 C10 C9 . . 124.0(3) ?
N2 C10 H10 . . 118.0 ?
C9 C10 H10 . . 118.0 ?
N2 C11 C12 . . 123.4(3) ?
N2 C11 H11 . . 118.3 ?
C12 C11 H11 . . 118.3 ?
C11 C12 C8 . . 119.3(3) ?
C11 C12 H12 . . 120.3 ?
C8 C12 H12 . . 120.3 ?
N6 C13 N5 . . 125.1(3) ?
N6 C13 C14 . . 117.8(3) ?
N5 C13 C14 . . 117.1(3) ?
C18 C14 C15 . . 118.2(3) ?
C18 C14 C13 . . 120.7(3) ?
C15 C14 C13 . . 121.1(3) ?
C14 C15 C16 . . 117.9(4) ?
C14 C15 H15 . . 121.1 ?
C16 C15 H15 . . 121.1 ?
N3 C16 C15 . . 124.6(4) ?
N3 C16 H16 . . 117.7 ?
C15 C16 H16 . . 117.7 ?
N3 C17 C18 . . 124.7(4) ?
N3 C17 H17 . . 117.7 ?
C18 C17 H17 . . 117.7 ?
C14 C18 C17 . . 118.6(4) ?
C14 C18 H18 . . 120.7 ?
C17 C18 H18 . . 120.7 ?
N7 C19 S1 . . 178.5(3) yes
O1 C20 H20A . . 109.5 ?
O1 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
O1 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
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
O1 HO1 N2 2_555 0.96 1.77 2.721(4) 173 yes
_cod_database_fobs_code 2013000