#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/65/2226517.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_2226517
loop_
_publ_author_name
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Poly[[bis(μ-4,4'-bipyridyl-κ²N:N')bis(thiocyanato-κN)manganese(II)]
 diethyl ether disolvate]
;
_journal_coeditor_code           HY2314
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m781
_journal_paper_doi               10.1107/S1600536810021665
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mn (N C S)2 (C10 H8 N2)2], 2C4 H10 O'
_chemical_formula_moiety         'C22 H16 Mn N6 S2, 2(C4 H10 O)'
_chemical_formula_sum            'C30 H36 Mn N6 O2 S2'
_chemical_formula_weight         631.71
_chemical_name_systematic
;
Poly[[bis(μ-4,4'-bipyridyl-κ²N:N')bis(thiocyanato-
κN)manganese(II)] diethyl ether disolvate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 106.75(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.702(2)
_cell_length_b                   11.6391(18)
_cell_length_c                   13.424(2)
_cell_measurement_reflns_used    11086
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.36
_cell_volume                     1750.8(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_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      230(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'ω 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  0.1336
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11086
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.724
_refine_diff_density_min         -1.367
_refine_ls_extinction_coef       0.034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0726
_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)+(0.1115P)²+1.3719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2056
_reflns_number_gt                2446
_reflns_number_total             2954
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2314.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2226517
_cod_database_fobs_code          2226517
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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 0.71119(6) 0.7500 0.0284(3) Uani d S 1 . .
N N1 0.3018(2) 0.7070(3) 0.7479(3) 0.0385(8) Uani d . 1 . .
C C1 0.2710(3) 0.6632(5) 0.8264(4) 0.0557(13) Uani d . 1 . .
H H1 0.3317 0.6340 0.8829 0.067 Uiso calc R 1 . .
C C2 0.1544(4) 0.6575(5) 0.8310(4) 0.0617(15) Uani d . 1 . .
H H2 0.1373 0.6249 0.8892 0.074 Uiso calc R 1 . .
C C3 0.0633(3) 0.7003(4) 0.7491(4) 0.0408(10) Uani d . 1 . .
C C4 0.0940(3) 0.7447(5) 0.6646(4) 0.0577(13) Uani d . 1 . .
H H4 0.0352 0.7725 0.6061 0.069 Uiso calc R 1 . .
C C5 0.2141(3) 0.7470(5) 0.6684(4) 0.0559(13) Uani d . 1 . .
H H5 0.2346 0.7788 0.6115 0.067 Uiso calc R 1 . .
N N11 0.5000 0.9088(4) 0.7500 0.0367(11) Uani d S 1 . .
N N12 0.5000 1.5156(3) 0.7500 0.0354(11) Uani d S 1 . .
C C11 0.4781(4) 0.9689(3) 0.8272(4) 0.0448(10) Uani d . 1 . .
H H11 0.4624 0.9285 0.8824 0.054 Uiso calc R 1 . .
C C12 0.4775(4) 1.0865(4) 0.8300(4) 0.0498(11) Uani d . 1 . .
H H12 0.4619 1.1249 0.8862 0.060 Uiso calc R 1 . .
C C13 0.5000 1.1484(4) 0.7500 0.0384(13) Uani d S 1 . .
C C16 0.4344(4) 1.4556(4) 0.6684(4) 0.0488(11) Uani d . 1 . .
H H16 0.3880 1.4963 0.6104 0.059 Uiso calc R 1 . .
C C15 0.4314(4) 1.3368(4) 0.6652(4) 0.0509(11) Uani d . 1 . .
H H17 0.3837 1.2982 0.6063 0.061 Uiso calc R 1 . .
C C14 0.5000 1.2758(4) 0.7500 0.0390(13) Uani d S 1 . .
N N21 0.5534(3) 0.7169(3) 0.9196(3) 0.0386(8) Uani d . 1 . .
C C21 0.6253(3) 0.6927(3) 0.9963(4) 0.0412(10) Uani d . 1 . .
S S21 0.72754(14) 0.65840(19) 1.10210(13) 0.0900(6) Uani d . 1 . .
C C31 0.0822(10) 0.3656(13) 0.6206(10) 0.170(6) Uani d . 1 . .
H H31A 0.1479 0.4018 0.6020 0.255 Uiso calc R 1 . .
H H31B 0.0756 0.3981 0.6853 0.255 Uiso calc R 1 . .
H H31C 0.0086 0.3787 0.5659 0.255 Uiso calc R 1 . .
C C32 0.1059(12) 0.2324(15) 0.6347(9) 0.172(6) Uani d . 1 . .
H H32A 0.1679 0.2177 0.7002 0.206 Uiso calc R 1 . .
H H32B 0.0329 0.1930 0.6375 0.206 Uiso calc R 1 . .
O O31 0.1431(5) 0.1896(8) 0.5502(5) 0.138(3) Uani d . 1 . .
C C33 0.1686(9) 0.0670(10) 0.5534(11) 0.146(5) Uani d . 1 . .
H H33A 0.0974 0.0238 0.5554 0.175 Uiso calc R 1 . .
H H33B 0.2328 0.0489 0.6166 0.175 Uiso calc R 1 . .
C C34 0.2049(11) 0.0329(12) 0.4606(12) 0.167(5) Uani d . 1 . .
H H34A 0.1368 0.0383 0.3991 0.251 Uiso calc R 1 . .
H H34B 0.2341 -0.0456 0.4688 0.251 Uiso calc R 1 . .
H H34C 0.2676 0.0837 0.4530 0.251 Uiso calc R 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'
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
N21 Mn1 N21 . 2_656 176.54(16) ?
N21 Mn1 N12 . 1_545 91.73(8) ?
N21 Mn1 N12 2_656 1_545 91.73(8) ?
N21 Mn1 N11 . . 88.27(8) ?
N21 Mn1 N11 2_656 . 88.27(8) ?
N12 Mn1 N11 1_545 . 180.0 ?
N21 Mn1 N1 . . 89.88(12) ?
N21 Mn1 N1 2_656 . 90.19(12) ?
N12 Mn1 N1 1_545 . 88.79(8) ?
N11 Mn1 N1 . . 91.21(8) ?
N21 Mn1 N1 . 2_656 90.19(12) ?
N21 Mn1 N1 2_656 2_656 89.88(12) ?
N12 Mn1 N1 1_545 2_656 88.79(8) ?
N11 Mn1 N1 . 2_656 91.21(8) ?
N1 Mn1 N1 . 2_656 177.58(16) ?
C1 N1 C5 . . 116.9(3) ?
C1 N1 Mn1 . . 120.3(3) ?
C5 N1 Mn1 . . 122.7(3) ?
N1 C1 C2 . . 123.8(4) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C1 C2 C3 . . 119.4(4) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 117.5(3) ?
C4 C3 C3 . 2_556 120.5(4) ?
C2 C3 C3 . 2_556 122.0(5) ?
C3 C4 C5 . . 118.4(4) ?
C3 C4 H4 . . 120.8 ?
C5 C4 H4 . . 120.8 ?
N1 C5 C4 . . 124.0(4) ?
N1 C5 H5 . . 118.0 ?
C4 C5 H5 . . 118.0 ?
C11 N11 C11 . 2_656 116.8(5) ?
C11 N11 Mn1 . . 121.6(2) ?
C11 N11 Mn1 2_656 . 121.6(2) ?
C16 N12 C16 . 2_656 117.1(5) ?
C16 N12 Mn1 . 1_565 121.4(2) ?
C16 N12 Mn1 2_656 1_565 121.4(2) ?
N11 C11 C12 . . 123.3(4) ?
N11 C11 H11 . . 118.4 ?
C12 C11 H11 . . 118.4 ?
C11 C12 C13 . . 119.8(4) ?
C11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
C12 C13 C12 . 2_656 117.0(5) ?
C12 C13 C14 . . 121.5(3) ?
C12 C13 C14 2_656 . 121.5(3) ?
N12 C16 C15 . . 123.4(4) ?
N12 C16 H16 . . 118.3 ?
C15 C16 H16 . . 118.3 ?
C16 C15 C14 . . 118.9(4) ?
C16 C15 H17 . . 120.6 ?
C14 C15 H17 . . 120.6 ?
C15 C14 C15 2_656 . 118.3(5) ?
C15 C14 C13 2_656 . 120.8(3) ?
C15 C14 C13 . . 120.8(3) ?
C21 N21 Mn1 . . 146.6(3) ?
N21 C21 S21 . . 178.9(4) ?
C32 C31 H31A . . 109.5 ?
C32 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C32 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
O31 C32 C31 . . 109.5(10) ?
O31 C32 H32A . . 109.8 ?
C31 C32 H32A . . 109.8 ?
O31 C32 H32B . . 109.8 ?
C31 C32 H32B . . 109.8 ?
H32A C32 H32B . . 108.2 ?
C32 O31 C33 . . 115.3(10) ?
O31 C33 C34 . . 110.1(10) ?
O31 C33 H33A . . 109.6 ?
C34 C33 H33A . . 109.6 ?
O31 C33 H33B . . 109.6 ?
C34 C33 H33B . . 109.6 ?
H33A C33 H33B . . 108.2 ?
C33 C34 H34A . . 109.5 ?
C33 C34 H34B . . 109.5 ?
H34A C34 H34B . . 109.5 ?
C33 C34 H34C . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 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
Mn1 N21 . 2.181(4) y
Mn1 N12 1_545 2.277(4) y
Mn1 N11 . 2.300(4) y
Mn1 N1 . 2.312(3) y
N1 C1 . 1.311(6) ?
N1 C5 . 1.333(6) ?
C1 C2 . 1.385(5) ?
C1 H1 . 0.9400 ?
C2 C3 . 1.386(6) ?
C2 H2 . 0.9400 ?
C3 C4 . 1.384(7) ?
C3 C3 2_556 1.488(6) ?
C4 C5 . 1.392(5) ?
C4 H4 . 0.9400 ?
C5 H5 . 0.9400 ?
N11 C11 . 1.334(5) ?
N11 C11 2_656 1.334(5) ?
N12 C16 . 1.338(5) ?
N12 C16 2_656 1.338(5) ?
N12 Mn1 1_565 2.277(4) ?
C11 C12 . 1.370(6) ?
C11 H11 . 0.9400 ?
C12 C13 . 1.380(5) ?
C12 H12 . 0.9400 ?
C13 C12 2_656 1.380(5) ?
C13 C14 . 1.483(7) ?
C16 C15 . 1.383(6) ?
C16 H16 . 0.9400 ?
C15 C14 . 1.385(5) ?
C15 H17 . 0.9400 ?
C14 C15 2_656 1.385(5) ?
N21 C21 . 1.161(6) ?
C21 S21 . 1.621(5) ?
C31 C32 . 1.577(18) ?
C31 H31A . 0.9700 ?
C31 H31B . 0.9700 ?
C31 H31C . 0.9700 ?
C32 O31 . 1.418(13) ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
O31 C33 . 1.455(12) ?
C33 C34 . 1.482(16) ?
C33 H33A . 0.9800 ?
C33 H33B . 0.9800 ?
C34 H34A . 0.9700 ?
C34 H34B . 0.9700 ?
C34 H34C . 0.9700 ?
