#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/63/2226374.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_2226374
loop_
_publ_author_name
'Wang, Fu-Ming'
_publ_section_title
;
 {N,N'-Bis[1-(2-pyridyl)ethylidene]ethane-1,2-diamine-κ⁴N,N',N'',N'''}bis(thiocyanato-κN)manganese(II)
;
_journal_coeditor_code           CI5097
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m776
_journal_paper_doi               10.1107/S1600536810021550
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mn (N C S)2 (C16 H18 N4)]'
_chemical_formula_moiety         'C18 H18 Mn N6 S2'
_chemical_formula_sum            'C18 H18 Mn N6 S2'
_chemical_formula_weight         437.44
_chemical_name_systematic
;
{N,N'-Bis[1-(2-pyridyl)ethylidene]ethane-1,2-diamine-
κ⁴N,N',N'',N'''}bis(thiocyanato-
κN)manganese(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 90.857(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.570(4)
_cell_length_b                   16.341(5)
_cell_length_c                   9.962(3)
_cell_measurement_reflns_used    1222
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.6
_cell_volume                     2046.0(11)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'ω 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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4479
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8813
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0388
_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)+(0.0354P)²+1.1621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                1590
_reflns_number_total             2173
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci5097.cif
_cod_data_source_block           I
_cod_original_cell_volume        2045.9(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2226374
_cod_database_fobs_code          2226374
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'
'-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_type_symbol
_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
Mn Mn1 0.5000 0.28864(3) 0.2500 0.04525(18) Uani d S 1 . .
N N1 0.42596(16) 0.32743(14) 0.03855(19) 0.0533(5) Uani d . 1 . .
N N2 0.44344(15) 0.17790(12) 0.13277(18) 0.0471(5) Uani d . 1 . .
N N3 0.63772(18) 0.34541(15) 0.1706(2) 0.0648(6) Uani d . 1 . .
S S1 0.82249(6) 0.38624(6) 0.04009(8) 0.0872(3) Uani d . 1 . .
C C1 0.4168(2) 0.40396(19) -0.0058(3) 0.0700(8) Uani d . 1 . .
H H1 0.4354 0.4463 0.0523 0.084 Uiso calc R 1 . .
C C2 0.3812(2) 0.4238(2) -0.1337(3) 0.0770(9) Uani d . 1 . .
H H2 0.3750 0.4781 -0.1605 0.092 Uiso calc R 1 . .
C C3 0.3554(2) 0.3616(2) -0.2193(3) 0.0774(9) Uani d . 1 . .
H H3 0.3325 0.3729 -0.3065 0.093 Uiso calc R 1 . .
C C4 0.3636(2) 0.28185(19) -0.1753(3) 0.0658(8) Uani d . 1 . .
H H4 0.3455 0.2388 -0.2323 0.079 Uiso calc R 1 . .
C C5 0.39910(18) 0.26645(16) -0.0454(2) 0.0492(6) Uani d . 1 . .
C C6 0.40708(18) 0.18264(16) 0.0130(2) 0.0482(6) Uani d . 1 . .
C C7 0.3715(2) 0.11213(18) -0.0729(3) 0.0731(8) Uani d . 1 . .
H H7A 0.4227 0.1028 -0.1418 0.110 Uiso calc R 1 . .
H H7B 0.3036 0.1246 -0.1134 0.110 Uiso calc R 1 . .
H H7C 0.3654 0.0639 -0.0184 0.110 Uiso calc R 1 . .
C C8 0.4512(2) 0.10020(15) 0.2047(2) 0.0563(7) Uani d . 1 . .
H H8A 0.4556 0.0555 0.1410 0.068 Uiso calc R 1 . .
H H8B 0.3881 0.0922 0.2580 0.068 Uiso calc R 1 . .
C C9 0.7137(2) 0.36210(16) 0.1152(2) 0.0515(6) Uani d . 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Mn1 N3 . 2_655 128.28(13) ?
N3 Mn1 N2 . . 114.09(8) ?
N3 Mn1 N2 2_655 . 106.83(8) ?
N3 Mn1 N2 . 2_655 106.83(8) ?
N3 Mn1 N2 2_655 2_655 114.09(8) ?
N2 Mn1 N2 . 2_655 73.78(10) ?
N3 Mn1 N1 . 2_655 84.43(8) ?
N3 Mn1 N1 2_655 2_655 82.20(8) ?
N2 Mn1 N1 . 2_655 141.89(7) ?
N2 Mn1 N1 2_655 2_655 68.89(7) ?
N3 Mn1 N1 . . 82.20(8) ?
N3 Mn1 N1 2_655 . 84.43(8) ?
N2 Mn1 N1 . . 68.89(7) ?
N2 Mn1 N1 2_655 . 141.89(7) ?
N1 Mn1 N1 2_655 . 149.06(11) ?
C1 N1 C5 . . 118.1(2) ?
C1 N1 Mn1 . . 125.15(18) ?
C5 N1 Mn1 . . 116.51(16) ?
C6 N2 C8 . . 122.2(2) ?
C6 N2 Mn1 . . 122.72(17) ?
C8 N2 Mn1 . . 115.07(14) ?
C9 N3 Mn1 . . 166.9(2) ?
N1 C1 C2 . . 123.5(3) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C3 C2 C1 . . 118.2(3) ?
C3 C2 H2 . . 120.9 ?
C1 C2 H2 . . 120.9 ?
C2 C3 C4 . . 119.4(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.3(3) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
N1 C5 C4 . . 121.5(2) ?
N1 C5 C6 . . 115.1(2) ?
C4 C5 C6 . . 123.4(2) ?
N2 C6 C5 . . 116.3(2) ?
N2 C6 C7 . . 126.0(2) ?
C5 C6 C7 . . 117.7(2) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
N2 C8 C8 . 2_655 109.89(15) ?
N2 C8 H8A . . 109.7 ?
C8 C8 H8A 2_655 . 109.7 ?
N2 C8 H8B . . 109.7 ?
C8 C8 H8B 2_655 . 109.7 ?
H8A C8 H8B . . 108.2 ?
N3 C9 S1 . . 178.7(2) ?
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
Mn1 N3 . 2.127(2) y
Mn1 N3 2_655 2.127(2) ?
Mn1 N2 . 2.263(2) y
Mn1 N2 2_655 2.263(2) ?
Mn1 N1 2_655 2.376(2) ?
Mn1 N1 . 2.376(2) y
N1 C1 . 1.331(3) ?
N1 C5 . 1.341(3) ?
N2 C6 . 1.273(3) ?
N2 C8 . 1.461(3) ?
N3 C9 . 1.144(3) ?
S1 C9 . 1.617(3) ?
C1 C2 . 1.382(4) ?
C1 H1 . 0.93 ?
C2 C3 . 1.363(4) ?
C2 H2 . 0.93 ?
C3 C4 . 1.378(4) ?
C3 H3 . 0.93 ?
C4 C5 . 1.386(3) ?
C4 H4 . 0.93 ?
C5 C6 . 1.491(4) ?
C6 C7 . 1.500(3) ?
C7 H7A . 0.96 ?
C7 H7B . 0.96 ?
C7 H7C . 0.96 ?
C8 C8 2_655 1.512(5) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
