#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:36:18 +0100 (vie 25 de mar de 2016) $
#$Revision: 179798 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/94/7009415.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_7009415
loop_
_publ_author_name
'Barandika, M. Gotzone'
'Hernández-Pino, Margarita L.'
'Urtiaga, M. Karmele'
'Cortés, Roberto'
'Lezama, Luis'
'Arriortua, M. Isabel'
'Rojo, Teófilo'
_publ_section_title
;
 Solvent control in the synthesis of [Mn(NCS)2(bpe)2(H2O)2] and
 [Mn(NCS)2(bpe)1.5(CH3OH)]n
 (bpe = 1,2-bis(4-pyridyl)ethene): structural analysis
 and magnetic properties
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1469
_journal_paper_doi               10.1039/b000808g
_journal_year                    2000
_chemical_formula_sum            'C21 H18 Mn N5 O S2'
_chemical_formula_weight         475.46
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                114.500(10)
_cell_angle_beta                 92.070(10)
_cell_angle_gamma                93.870(10)
_cell_formula_units_Z            2
_cell_length_a                   8.807(2)
_cell_length_b                   11.130(2)
_cell_length_c                   12.9720(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1151.5(4)
_computing_cell_refinement       'Enraf-Nonius CAD-4'
_computing_data_collection       'Enraf-Nonius CAD-4'
_computing_data_reduction        'Xtal 3.2 (Hall, Flack & Stewart, 1992)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6709
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.73
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.776
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_F_000             488
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.663
_refine_ls_goodness_of_fit_obs   0.548
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6709
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.663
_refine_ls_restrained_S_obs      0.548
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_obs          0.0481
_refine_ls_shift/esd_max         -1.468
_refine_ls_shift/esd_mean        0.081
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2478P)²+1.6471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2361
_refine_ls_wR_factor_obs         0.1594
_reflns_number_observed          4341
_reflns_number_total             6709
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000808g.txt
_cod_data_source_block           mnncs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2478P)^2^+1.6471P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2478P)^2^+1.6471P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1151.5(3)
_cod_database_code               7009415
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn -0.06913(5) 0.42880(4) 0.18844(4) 0.0354(2) Uani 1 d . .
N4 N -0.1882(4) 0.2829(3) 0.2329(3) 0.0533(8) Uani 1 d . .
C19 C -0.2779(5) 0.2333(4) 0.2685(3) 0.0517(8) Uani 1 d . .
S1A S -0.4201(12) 0.1812(13) 0.3208(8) 0.091(3) Uani 0.50 d P .
S1B S -0.3872(12) 0.1510(13) 0.3181(10) 0.099(3) Uani 0.50 d P .
N5 N 0.0395(4) 0.5795(3) 0.1418(3) 0.0499(7) Uani 1 d . .
C20 C 0.1021(4) 0.6362(3) 0.0960(3) 0.0375(6) Uani 1 d . .
S2 S 0.19327(12) 0.71391(10) 0.03046(8) 0.0499(2) Uani 1 d . .
N1 N 0.1347(3) 0.3075(3) 0.1370(3) 0.0419(6) Uani 1 d . .
C1 C 0.1156(4) 0.1757(4) 0.1062(4) 0.0514(9) Uani 1 d . .
H1 H 0.0201(4) 0.1388(4) 0.1120(4) 0.096(5) Uiso 1 calc R .
C2 C 0.2293(4) 0.0930(3) 0.0668(4) 0.0517(9) Uani 1 d . .
H2 H 0.2098(4) 0.0025(3) 0.0462(4) 0.096(5) Uiso 1 calc R .
C3 C 0.3741(4) 0.1450(3) 0.0577(3) 0.0400(6) Uani 1 d . .
C4 C 0.3947(4) 0.2811(3) 0.0918(4) 0.0499(8) Uani 1 d . .
H4 H 0.4896(4) 0.3211(3) 0.0888(4) 0.096(5) Uiso 1 calc R .
C5 C 0.2731(4) 0.3574(3) 0.1302(4) 0.0506(8) Uani 1 d . .
H5 H 0.2895(4) 0.4484(3) 0.1523(4) 0.096(5) Uiso 1 calc R .
C6 C 0.5024(4) 0.0645(3) 0.0176(3) 0.0442(7) Uani 1 d D .
H6 H 0.6071(31) 0.1113(55) 0.0240(53) 0.096(5) Uiso 1 d D .
N2 N -0.2787(3) 0.5465(3) 0.2303(3) 0.0464(6) Uani 1 d . .
C7 C -0.3235(5) 0.6129(4) 0.1702(4) 0.0627(11) Uani 1 d . .
H7 H -0.2783(5) 0.5987(4) 0.1029(4) 0.096(5) Uiso 1 calc R .
C8 C -0.4333(6) 0.7009(5) 0.2040(6) 0.089(2) Uani 1 d . .
H8 H -0.4627(6) 0.7420(5) 0.1579(6) 0.096(5) Uiso 1 calc R .
C9 C -0.5001(5) 0.7292(5) 0.3043(6) 0.088(2) Uani 1 d . .
C10 C -0.4554(5) 0.6584(5) 0.3652(5) 0.077(2) Uani 1 d . .
H10 H -0.4991(5) 0.6715(5) 0.4329(5) 0.096(5) Uiso 1 calc R .
C11 C -0.3469(4) 0.5690(4) 0.3265(4) 0.0554(9) Uani 1 d . .
H11 H -0.3201(4) 0.5226(4) 0.3688(4) 0.096(5) Uiso 1 calc R .
C12A C -0.5995(8) 0.8408(7) 0.3163(6) 0.0441(14) Uani 0.50 d P .
C13A C -0.6618(8) 0.8933(7) 0.4173(7) 0.0451(15) Uani 0.50 d P .
C13B C -0.6604(9) 0.9037(8) 0.3438(7) 0.049(2) Uani 0.50 d P .
C12B C -0.6118(9) 0.8212(9) 0.3839(8) 0.052(2) Uani 0.50 d P .
C14 C -0.9094(6) 1.1694(5) 0.4145(5) 0.0705(12) Uani 1 d . .
H14 H -0.9485(6) 1.2089(5) 0.3698(5) 0.096(5) Uiso 1 calc R .
C15 C -0.8184(7) 1.0684(5) 0.3661(6) 0.089(2) Uani 1 d . .
H15 H -0.7957(7) 1.0420(5) 0.2908(6) 0.096(5) Uiso 1 calc R .
C16 C -0.7600(5) 1.0052(4) 0.4293(6) 0.088(2) Uani 1 d . .
C17 C -0.7996(5) 1.0504(4) 0.5399(6) 0.080(2) Uani 1 d . .
H17 H -0.7646(5) 1.0110(4) 0.5859(6) 0.096(5) Uiso 1 calc R .
C18 C -0.8904(5) 1.1529(4) 0.5829(4) 0.0593(10) Uani 1 d . .
H18 H -0.9150(5) 1.1810(4) 0.6579(4) 0.096(5) Uiso 1 calc R .
N3 N -0.9449(4) 1.2144(3) 0.5228(3) 0.0582(8) Uani 1 d . .
O1 O 0.0354(4) 0.5426(3) 0.3605(2) 0.0564(7) Uani 1 d D .
H100 H 0.0046(70) 0.6351(25) 0.4018(45) 0.096(5) Uiso 1 d D .
C21 C 0.1610(6) 0.5211(5) 0.4179(4) 0.0664(11) Uani 1 d . .
H211 H 0.1765(6) 0.5910(5) 0.4930(4) 0.096(5) Uiso 1 calc R .
H212 H 0.2504(6) 0.5198(5) 0.3773(4) 0.096(5) Uiso 1 calc R .
H213 H 0.1424(6) 0.4376(5) 0.4226(4) 0.096(5) Uiso 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'
Mn Mn 0.3368 0.7283 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
N4 Mn1 N5 176.97(13) . . ?
N4 Mn1 O1 93.38(13) . . ?
N5 Mn1 O1 87.88(12) . . ?
N4 Mn1 N1 91.90(12) . . ?
N5 Mn1 N1 90.83(12) . . ?
O1 Mn1 N1 91.60(11) . . ?
N4 Mn1 N2 88.57(13) . . ?
N5 Mn1 N2 88.64(13) . . ?
O1 Mn1 N2 91.35(11) . . ?
N1 Mn1 N2 176.98(11) . . ?
N4 Mn1 S2 87.71(10) . 2_565 ?
N5 Mn1 S2 91.09(9) . 2_565 ?
O1 Mn1 S2 178.46(9) . 2_565 ?
N1 Mn1 S2 87.28(8) . 2_565 ?
N2 Mn1 S2 89.76(8) . 2_565 ?
C19 N4 Mn1 160.8(3) . . ?
N4 C19 S1A 171.4(6) . . ?
N4 C19 S1B 172.6(6) . . ?
S1A C19 S1B 15.9(7) . . ?
C20 N5 Mn1 165.4(3) . . ?
N5 C20 S2 178.7(3) . . ?
C20 S2 Mn1 100.49(11) . 2_565 ?
C5 N1 C1 116.7(3) . . ?
C5 N1 Mn1 123.9(2) . . ?
C1 N1 Mn1 119.3(2) . . ?
N1 C1 C2 123.6(3) . . ?
C1 C2 C3 119.8(3) . . ?
C4 C3 C2 116.6(3) . . ?
C4 C3 C6 119.8(3) . . ?
C2 C3 C6 123.6(3) . . ?
C5 C4 C3 119.8(3) . . ?
N1 C5 C4 123.5(3) . . ?
C6 C6 C3 125.8(4) 2_655 . ?
C7 N2 C11 116.9(4) . . ?
C7 N2 Mn1 121.7(3) . . ?
C11 N2 Mn1 120.6(3) . . ?
N2 C7 C8 122.8(5) . . ?
C9 C8 C7 121.2(5) . . ?
C8 C9 C10 115.7(4) . . ?
C8 C9 C12A 104.7(6) . . ?
C10 C9 C12A 139.4(6) . . ?
C8 C9 C12B 142.4(6) . . ?
C10 C9 C12B 101.8(6) . . ?
C12A C9 C12B 37.7(4) . . ?
C11 C10 C9 120.8(5) . . ?
N2 C11 C10 122.5(5) . . ?
C13B C12A C12B 89.2(10) . . ?
C13B C12A C13A 48.2(7) . . ?
C12B C12A C13A 41.5(6) . . ?
C13B C12A C9 161.7(11) . . ?
C12B C12A C9 72.6(8) . . ?
C13A C12A C9 113.5(7) . . ?
C13B C13A C12B 87.3(9) . . ?
C13B C13A C12A 40.3(6) . . ?
C12B C13A C12A 47.6(7) . . ?
C13B C13A C16 73.1(7) . . ?
C12B C13A C16 159.3(11) . . ?
C12A C13A C16 113.4(7) . . ?
C12A C13B C13A 91.5(9) . . ?
C12A C13B C12B 49.2(7) . . ?
C13A C13B C12B 42.8(6) . . ?
C12A C13B C16 160.3(11) . . ?
C13A C13B C16 68.8(7) . . ?
C12B C13B C16 111.3(8) . . ?
C12A C12B C13A 90.9(9) . . ?
C12A C12B C13B 41.6(6) . . ?
C13A C12B C13B 49.9(7) . . ?
C12A C12B C9 69.7(8) . . ?
C13A C12B C9 158.3(11) . . ?
C13B C12B C9 111.2(8) . . ?
N3 C14 C15 123.4(5) . . ?
C14 C15 C16 120.1(6) . . ?
C17 C16 C15 116.1(4) . . ?
C17 C16 C13A 103.3(6) . . ?
C15 C16 C13A 140.6(6) . . ?
C17 C16 C13B 141.2(6) . . ?
C15 C16 C13B 102.6(6) . . ?
C13A C16 C13B 38.1(4) . . ?
C16 C17 C18 120.5(5) . . ?
N3 C18 C17 123.4(5) . . ?
C18 N3 C14 116.5(4) . . ?
C21 O1 Mn1 131.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N4 2.159(3) . ?
Mn1 N5 2.182(3) . ?
Mn1 O1 2.186(3) . ?
Mn1 N1 2.271(3) . ?
Mn1 N2 2.286(3) . ?
Mn1 S2 2.7535(11) 2_565 ?
N4 C19 1.149(5) . ?
C19 S1A 1.630(10) . ?
C19 S1B 1.610(10) . ?
N5 C20 1.158(4) . ?
C20 S2 1.637(3) . ?
S2 Mn1 2.7536(11) 2_565 ?
N1 C5 1.326(4) . ?
N1 C1 1.347(4) . ?
C1 C2 1.373(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.388(5) . ?
C3 C6 1.463(4) . ?
C4 C5 1.388(5) . ?
C6 C6 1.312(7) 2_655 ?
N2 C7 1.343(5) . ?
N2 C11 1.340(5) . ?
C7 C8 1.374(6) . ?
C8 C9 1.371(10) . ?
C9 C10 1.393(9) . ?
C9 C12A 1.526(8) . ?
C9 C12B 1.554(10) . ?
C10 C11 1.380(6) . ?
C12A C13B 0.873(9) . ?
C12A C12B 0.996(11) . ?
C12A C13A 1.349(10) . ?
C13A C13B 1.006(11) . ?
C13A C12B 0.894(10) . ?
C13A C16 1.522(8) . ?
C13B C12B 1.315(10) . ?
C13B C16 1.562(10) . ?
C14 N3 1.338(6) . ?
C14 C15 1.368(7) . ?
C15 C16 1.388(10) . ?
C16 C17 1.377(9) . ?
C17 C18 1.371(6) . ?
C18 N3 1.329(6) . ?
O1 C21 1.400(5) . ?
