#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$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
trans-Bis(isothiocyanato-κN)bis(methanol-κO)bis[2,4,6-tri(4-pyridyl)-1,3,5-triazine-κN²]manganese(II)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m521
_journal_page_last               m522
_journal_paper_doi               10.1107/S0108270102016475
_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-\kN⁴]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       θ/2θ
_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      ?
_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/[σ²(Fo²)+(0.0374P)²+1.8244P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            ob1080.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1015.3(4)
_cod_database_code               2013000
_cod_database_fobs_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_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_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_
_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
