#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/02/2240274.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_2240274
loop_
_publ_author_name
'Suckert, Stefan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 bis(2,2'-bipyridine-κ²N,N')bis(thiocyanato-κN)manganese(II)
 2,2'-bipyridine monosolvate
;
_journal_coeditor_code           WM5090
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3
_journal_page_last               m4
_journal_paper_doi               10.1107/S205698901402516X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Mn (N C S)2 (C10 H8 N2)2], C10 H8 N2'
_chemical_formula_moiety         'C22 H16 Mn N6 S2, C10 H8 N2'
_chemical_formula_sum            'C32 H24 Mn N8 S2'
_chemical_formula_weight         639.65
_chemical_name_systematic
'Bis(2,2'-bipyridine-κ²N,N')bis(thiocyanato-κN)manganese(II) 2,2'-bipyridine monosolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.535(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5263(6)
_cell_length_b                   13.5383(4)
_cell_length_c                   16.0726(7)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.45
_cell_volume                     3045.4(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-2'
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41565
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.349
_refine_ls_extinction_coef       0.0025(9)
_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   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0405
_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)+(0.0384P)²+0.9654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                5766
_reflns_number_total             6630
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5090sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2240274
_cod_database_fobs_code          2240274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
Mn Mn1 0.734793(17) 0.128336(19) 0.478914(17) 0.04106(9) Uani d . 1 1
N N1 0.70830(14) 0.02009(14) 0.37737(12) 0.0665(5) Uani d . 1 1
C C1 0.71894(13) -0.04547(14) 0.33491(12) 0.0502(4) Uani d . 1 1
S S1 0.73507(5) -0.13676(5) 0.27623(4) 0.0792(2) Uani d . 1 1
N N2 0.75999(12) 0.02533(13) 0.58481(11) 0.0583(4) Uani d . 1 1
C C2 0.77308(12) -0.03438(13) 0.63794(12) 0.0453(4) Uani d . 1 1
S S2 0.79008(5) -0.11880(5) 0.71196(4) 0.07089(17) Uani d . 1 1
N N10 0.88949(10) 0.14680(12) 0.47586(10) 0.0513(4) Uani d . 1 1
C C10 0.92943(15) 0.09366(18) 0.42424(15) 0.0652(6) Uani d . 1 1
H H10 0.8898 0.0546 0.3818 0.078 Uiso calc R 1 1
C C11 1.02539(17) 0.0938(2) 0.43073(19) 0.0824(8) Uani d . 1 1
H H11 1.0502 0.0572 0.3928 0.099 Uiso calc R 1 1
C C12 1.08341(17) 0.1492(2) 0.4943(2) 0.0908(9) Uani d . 1 1
H H12 1.1490 0.1497 0.5010 0.109 Uiso calc R 1 1
C C13 1.04482(15) 0.2043(2) 0.54863(18) 0.0792(7) Uani d . 1 1
H H13 1.0840 0.2420 0.5924 0.095 Uiso calc R 1 1
C C14 0.94611(13) 0.20298(15) 0.53718(13) 0.0541(5) Uani d . 1 1
C C15 0.89768(13) 0.26359(14) 0.58963(12) 0.0517(4) Uani d . 1 1
C C16 0.94487(18) 0.33141(19) 0.65064(15) 0.0728(6) Uani d . 1 1
H H16 1.0108 0.3385 0.6629 0.087 Uiso calc R 1 1
C C17 0.8933(2) 0.3882(2) 0.69288(16) 0.0852(8) Uani d . 1 1
H H17 0.9244 0.4343 0.7337 0.102 Uiso calc R 1 1
C C18 0.7964(2) 0.37728(17) 0.67522(16) 0.0771(7) Uani d . 1 1
H H18 0.7605 0.4157 0.7030 0.092 Uiso calc R 1 1
C C19 0.75380(16) 0.30723(16) 0.61475(13) 0.0607(5) Uani d . 1 1
H H19 0.6880 0.2987 0.6025 0.073 Uiso calc R 1 1
N N11 0.80238(10) 0.25125(11) 0.57302(10) 0.0488(3) Uani d . 1 1
N N20 0.67171(10) 0.24892(11) 0.38090(9) 0.0470(3) Uani d . 1 1
C C20 0.72036(15) 0.29317(17) 0.33176(14) 0.0624(5) Uani d . 1 1
H H20 0.7831 0.2736 0.3374 0.075 Uiso calc R 1 1
C C21 0.68249(19) 0.36615(18) 0.27327(15) 0.0726(6) Uani d . 1 1
H H21 0.7188 0.3955 0.2404 0.087 Uiso calc R 1 1
C C22 0.59047(19) 0.39454(17) 0.26467(14) 0.0713(6) Uani d . 1 1
H H22 0.5632 0.4443 0.2260 0.086 Uiso calc R 1 1
C C24 0.58074(12) 0.27636(13) 0.37188(11) 0.0446(4) Uani d . 1 1
C C25 0.53069(12) 0.22504(13) 0.42834(11) 0.0438(4) Uani d . 1 1
C C26 0.43568(13) 0.24294(17) 0.42531(14) 0.0613(5) Uani d . 1 1
H H26 0.4000 0.2878 0.3858 0.074 Uiso calc R 1 1
C C27 0.39498(14) 0.19383(19) 0.48122(15) 0.0689(6) Uani d . 1 1
H H27 0.3314 0.2050 0.4797 0.083 Uiso calc R 1 1
C C28 0.44834(15) 0.12849(17) 0.53914(15) 0.0652(6) Uani d . 1 1
H H28 0.4223 0.0955 0.5782 0.078 Uiso calc R 1 1
C C29 0.54214(14) 0.11259(15) 0.53824(13) 0.0538(4) Uani d . 1 1
H H29 0.5782 0.0671 0.5768 0.065 Uiso calc R 1 1
N N21 0.58328(10) 0.15956(11) 0.48459(9) 0.0427(3) Uani d . 1 1
N N30 0.45727(13) 0.57292(15) 0.40356(13) 0.0690(5) Uani d . 1 1
C C30 0.52000(14) 0.52678(15) 0.46832(13) 0.0557(5) Uani d . 1 1
C C31 0.61789(15) 0.52953(17) 0.47611(15) 0.0654(5) Uani d . 1 1
H H31 0.6605 0.4974 0.5216 0.078 Uiso calc R 1 1
C C23 0.53780(16) 0.34899(15) 0.31364(13) 0.0597(5) Uani d . 1 1
H H23 0.4745 0.3668 0.3076 0.072 Uiso calc R 1 1
C C32 0.65066(18) 0.5801(2) 0.41603(18) 0.0766(6) Uani d . 1 1
H H32 0.7158 0.5826 0.4203 0.092 Uiso calc R 1 1
C C33 0.5866(2) 0.6271(2) 0.34934(19) 0.0813(7) Uani d . 1 1
H H33 0.6069 0.6617 0.3075 0.098 Uiso calc R 1 1
C C34 0.4917(2) 0.6212(2) 0.34664(18) 0.0822(7) Uani d . 1 1
H H34 0.4483 0.6533 0.3017 0.099 Uiso calc R 1 1
N N40 0.89931(14) 0.56056(16) 0.52370(14) 0.0753(5) Uani d . 1 1
C C40 0.99023(15) 0.53074(16) 0.53470(14) 0.0617(5) Uani d . 1 1
C C41 1.06105(17) 0.55483(19) 0.60838(17) 0.0756(6) Uani d . 1 1
H H41 1.1234 0.5332 0.6150 0.091 Uiso calc R 1 1
C C42 1.0391(2) 0.6106(2) 0.67145(19) 0.0877(8) Uani d . 1 1
H H42 1.0863 0.6269 0.7212 0.105 Uiso calc R 1 1
C C43 0.9471(2) 0.6423(2) 0.6607(2) 0.0887(8) Uani d . 1 1
H H43 0.9301 0.6808 0.7022 0.106 Uiso calc R 1 1
C C44 0.8805(2) 0.6148(2) 0.5856(2) 0.0891(8) Uani d . 1 1
H H44 0.8179 0.6360 0.5779 0.107 Uiso calc R 1 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_3
_geom_angle
N1 Mn1 N2 . 96.69(7)
N1 Mn1 N21 . 100.33(6)
N2 Mn1 N21 . 92.88(6)
N1 Mn1 N10 . 92.04(7)
N2 Mn1 N10 . 97.38(6)
N21 Mn1 N10 . 162.91(6)
N1 Mn1 N20 . 90.37(7)
N2 Mn1 N20 . 163.68(6)
N21 Mn1 N20 . 71.33(5)
N10 Mn1 N20 . 97.05(5)
N1 Mn1 N11 . 163.00(6)
N2 Mn1 N11 . 89.80(6)
N21 Mn1 N11 . 95.00(5)
N10 Mn1 N11 . 71.49(6)
N20 Mn1 N11 . 87.59(5)
C1 N1 Mn1 . 161.31(18)
N1 C1 S1 . 179.3(2)
C2 N2 Mn1 . 175.86(16)
N2 C2 S2 . 179.25(19)
C14 N10 C10 . 118.54(17)
C14 N10 Mn1 . 117.53(12)
C10 N10 Mn1 . 123.21(14)
N10 C10 C11 . 123.5(2)
N10 C10 H10 . 118.3
C11 C10 H10 . 118.3
C12 C11 C10 . 118.1(3)
C12 C11 H11 . 121.0
C10 C11 H11 . 121.0
C11 C12 C13 . 119.9(2)
C11 C12 H12 . 120.0
C13 C12 H12 . 120.0
C12 C13 C14 . 119.2(3)
C12 C13 H13 . 120.4
C14 C13 H13 . 120.4
N10 C14 C13 . 120.7(2)
N10 C14 C15 . 116.21(15)
C13 C14 C15 . 123.0(2)
N11 C15 C16 . 120.7(2)
N11 C15 C14 . 115.93(16)
C16 C15 C14 . 123.36(19)
C17 C16 C15 . 119.3(2)
C17 C16 H16 . 120.3
C15 C16 H16 . 120.3
C18 C17 C16 . 120.3(2)
C18 C17 H17 . 119.9
C16 C17 H17 . 119.9
C17 C18 C19 . 117.6(2)
C17 C18 H18 . 121.2
C19 C18 H18 . 121.2
N11 C19 C18 . 123.2(2)
N11 C19 H19 . 118.4
C18 C19 H19 . 118.4
C19 N11 C15 . 118.94(17)
C19 N11 Mn1 . 123.75(13)
C15 N11 Mn1 . 117.23(13)
C20 N20 C24 . 118.28(17)
C20 N20 Mn1 . 123.43(13)
C24 N20 Mn1 . 118.28(11)
N20 C20 C21 . 123.3(2)
N20 C20 H20 . 118.3
C21 C20 H20 . 118.3
C22 C21 C20 . 118.4(2)
C22 C21 H21 . 120.8
C20 C21 H21 . 120.8
C21 C22 C23 . 119.6(2)
C21 C22 H22 . 120.2
C23 C22 H22 . 120.2
N20 C24 C23 . 121.42(18)
N20 C24 C25 . 115.79(15)
C23 C24 C25 . 122.79(17)
N21 C25 C26 . 121.16(18)
N21 C25 C24 . 115.91(14)
C26 C25 C24 . 122.92(17)
C27 C26 C25 . 119.4(2)
C27 C26 H26 . 120.3
C25 C26 H26 . 120.3
C28 C27 C26 . 119.67(19)
C28 C27 H27 . 120.2
C26 C27 H27 . 120.2
C27 C28 C29 . 118.3(2)
C27 C28 H28 . 120.8
C29 C28 H28 . 120.8
N21 C29 C28 . 123.0(2)
N21 C29 H29 . 118.5
C28 C29 H29 . 118.5
C29 N21 C25 . 118.38(15)
C29 N21 Mn1 . 123.00(12)
C25 N21 Mn1 . 118.53(11)
C34 N30 C30 . 117.5(2)
N30 C30 C31 . 121.5(2)
N30 C30 C30 3_666 116.7(2)
C31 C30 C30 3_666 121.8(2)
C32 C31 C30 . 119.3(2)
C32 C31 H31 . 120.4
C30 C31 H31 . 120.4
C22 C23 C24 . 119.0(2)
C22 C23 H23 . 120.5
C24 C23 H23 . 120.5
C31 C32 C33 . 119.4(2)
C31 C32 H32 . 120.3
C33 C32 H32 . 120.3
C34 C33 C32 . 117.6(2)
C34 C33 H33 . 121.2
C32 C33 H33 . 121.2
N30 C34 C33 . 124.7(2)
N30 C34 H34 . 117.7
C33 C34 H34 . 117.7
C44 N40 C40 . 117.4(2)
N40 C40 C41 . 121.3(2)
N40 C40 C40 3_766 116.7(2)
C41 C40 C40 3_766 122.0(3)
C42 C41 C40 . 119.8(2)
C42 C41 H41 . 120.1
C40 C41 H41 . 120.1
C41 C42 C43 . 119.5(3)
C41 C42 H42 . 120.3
C43 C42 H42 . 120.3
C42 C43 C44 . 117.2(3)
C42 C43 H43 . 121.4
C44 C43 H43 . 121.4
N40 C44 C43 . 124.8(3)
N40 C44 H44 . 117.6
C43 C44 H44 . 117.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 N1 . 2.1501(18)
Mn1 N2 . 2.1546(17)
Mn1 N21 . 2.2669(13)
Mn1 N10 . 2.2746(14)
Mn1 N20 . 2.2833(15)
Mn1 N11 . 2.2859(15)
N1 C1 . 1.155(2)
C1 S1 . 1.609(2)
N2 C2 . 1.154(2)
C2 S2 . 1.6203(19)
N10 C14 . 1.339(3)
N10 C10 . 1.342(3)
C10 C11 . 1.370(3)
C10 H10 . 0.9300
C11 C12 . 1.362(4)
C11 H11 . 0.9300
C12 C13 . 1.377(4)
C12 H12 . 0.9300
C13 C14 . 1.396(3)
C13 H13 . 0.9300
C14 C15 . 1.482(3)
C15 N11 . 1.348(2)
C15 C16 . 1.384(3)
C16 C17 . 1.373(4)
C16 H16 . 0.9300
C17 C18 . 1.367(4)
C17 H17 . 0.9300
C18 C19 . 1.380(3)
C18 H18 . 0.9300
C19 N11 . 1.333(2)
C19 H19 . 0.9300
N20 C20 . 1.335(2)
N20 C24 . 1.343(2)
C20 C21 . 1.373(3)
C20 H20 . 0.9300
C21 C22 . 1.362(4)
C21 H21 . 0.9300
C22 C23 . 1.381(3)
C22 H22 . 0.9300
C24 C23 . 1.386(3)
C24 C25 . 1.479(2)
C25 N21 . 1.348(2)
C25 C26 . 1.389(2)
C26 C27 . 1.372(3)
C26 H26 . 0.9300
C27 C28 . 1.365(3)
C27 H27 . 0.9300
C28 C29 . 1.383(3)
C28 H28 . 0.9300
C29 N21 . 1.335(2)
C29 H29 . 0.9300
N30 C34 . 1.326(3)
N30 C30 . 1.340(3)
C30 C31 . 1.394(3)
C30 C30 3_666 1.489(4)
C31 C32 . 1.369(3)
C31 H31 . 0.9300
C23 H23 . 0.9300
C32 C33 . 1.373(4)
C32 H32 . 0.9300
C33 C34 . 1.370(4)
C33 H33 . 0.9300
C34 H34 . 0.9300
N40 C44 . 1.322(3)
N40 C40 . 1.347(3)
C40 C41 . 1.384(3)
C40 C40 3_766 1.479(5)
C41 C42 . 1.368(4)
C41 H41 . 0.9300
C42 C43 . 1.371(4)
C42 H42 . 0.9300
C43 C44 . 1.380(4)
C43 H43 . 0.9300
C44 H44 . 0.9300
