#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:39:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179487 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/84/4338467.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_4338467
loop_
_publ_author_name
'Hilbert, Jessica'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Influence of the Synthesis Parameters onto Nucleation and Crystallization
 of Five New Tin-Sulfur Containing Compounds.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5619
_journal_page_last               5630
_journal_paper_doi               10.1021/ic500369m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Sn2S6, Mn2C48H32N8'
_chemical_formula_sum            'C48 H32 Mn2 N8 S6 Sn2'
_chemical_formula_weight         1260.44
_chemical_name_common            '[Mn(phen)2]2Sn2S6'
_chemical_name_systematic        '[Mn(C12H8N2)2]2Sn2S6'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.356(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8230(4)
_cell_length_b                   9.8940(2)
_cell_length_c                   24.8107(10)
_cell_measurement_reflns_used    4449
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.62
_cell_measurement_theta_min      1.64
_cell_volume                     2656.05(15)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ 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  0.1060
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28028
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  0.8327
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0048(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0423
_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)+(0.0429P)²+2.4075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3840
_reflns_number_total             4449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500369m_si_002.cif
_cod_data_source_block           jh231
_cod_depositor_comments
'Adding full bibliography for 4338466--4338470.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4338467
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.12058(3) 0.43775(3) 0.036630(12) 0.04192(13) Uani 1 1 d .
S1 S 0.33375(10) 0.45707(11) 0.02451(5) 0.0474(3) Uani 1 1 d .
S2 S 0.11134(11) 0.30634(13) 0.11565(5) 0.0538(3) Uani 1 1 d .
S3 S -0.00020(12) 0.64680(11) 0.04050(5) 0.0524(3) Uani 1 1 d .
Mn1 Mn 0.34563(6) 0.30706(6) 0.10900(3) 0.04495(19) Uani 1 1 d .
N1 N 0.3714(4) 0.2115(4) 0.19664(17) 0.0506(9) Uani 1 1 d .
N2 N 0.4003(4) 0.4743(4) 0.16934(16) 0.0502(9) Uani 1 1 d .
C1 C 0.3533(5) 0.0847(5) 0.2112(2) 0.0586(13) Uani 1 1 d .
H1 H 0.3258 0.0239 0.1850 0.070 Uiso 1 1 calc R
C2 C 0.3725(6) 0.0370(5) 0.2630(3) 0.0700(15) Uani 1 1 d .
H2 H 0.3587 -0.0536 0.2708 0.084 Uiso 1 1 calc R
C3 C 0.4119(6) 0.1231(6) 0.3026(2) 0.0742(17) Uani 1 1 d .
H3 H 0.4265 0.0922 0.3375 0.089 Uiso 1 1 calc R
C4 C 0.4301(6) 0.2604(5) 0.2893(2) 0.0667(14) Uani 1 1 d .
C5 C 0.4671(8) 0.3591(6) 0.3286(2) 0.089(2) Uani 1 1 d .
H5 H 0.4820 0.3328 0.3641 0.107 Uiso 1 1 calc R
C6 C 0.4807(7) 0.4894(6) 0.3146(2) 0.089(2) Uani 1 1 d .
H6 H 0.5050 0.5520 0.3407 0.107 Uiso 1 1 calc R
C7 C 0.4586(6) 0.5335(5) 0.2607(2) 0.0667(15) Uani 1 1 d .
C8 C 0.4710(7) 0.6681(6) 0.2440(3) 0.086(2) Uani 1 1 d .
H8 H 0.4971 0.7339 0.2685 0.103 Uiso 1 1 calc R
C9 C 0.4452(7) 0.7022(6) 0.1926(3) 0.089(2) Uani 1 1 d .
H9 H 0.4501 0.7920 0.1819 0.107 Uiso 1 1 calc R
C10 C 0.4108(6) 0.6021(5) 0.1552(2) 0.0699(16) Uani 1 1 d .
H10 H 0.3951 0.6265 0.1195 0.084 Uiso 1 1 calc R
C11 C 0.4238(5) 0.4386(4) 0.2206(2) 0.0513(11) Uani 1 1 d .
C12 C 0.4085(4) 0.2997(4) 0.2361(2) 0.0497(11) Uani 1 1 d .
N11 N 0.3689(4) 0.0887(4) 0.08074(17) 0.0554(10) Uani 1 1 d .
N12 N 0.5538(3) 0.2673(4) 0.09926(17) 0.0517(10) Uani 1 1 d .
C21 C 0.2775(7) 0.0032(6) 0.0690(2) 0.0767(18) Uani 1 1 d .
H21 H 0.1961 0.0318 0.0718 0.092 Uiso 1 1 calc R
C22 C 0.3021(8) -0.1323(6) 0.0521(3) 0.087(2) Uani 1 1 d .
H22 H 0.2374 -0.1907 0.0432 0.104 Uiso 1 1 calc R
C23 C 0.4214(9) -0.1746(6) 0.0490(3) 0.086(2) Uani 1 1 d .
H23 H 0.4380 -0.2624 0.0379 0.103 Uiso 1 1 calc R
C24 C 0.5181(7) -0.0890(5) 0.0622(2) 0.0716(17) Uani 1 1 d .
C25 C 0.6465(8) -0.1262(7) 0.0597(3) 0.084(2) Uani 1 1 d .
H25 H 0.6668 -0.2145 0.0506 0.100 Uiso 1 1 calc R
C26 C 0.7362(7) -0.0390(7) 0.0699(3) 0.088(2) Uani 1 1 d .
H26 H 0.8178 -0.0678 0.0685 0.106 Uiso 1 1 calc R
C27 C 0.7105(6) 0.0990(6) 0.0830(2) 0.0693(15) Uani 1 1 d .
C28 C 0.8005(5) 0.1985(7) 0.0893(3) 0.0789(17) Uani 1 1 d .
H28 H 0.8835 0.1758 0.0866 0.095 Uiso 1 1 calc R
C29 C 0.7685(5) 0.3276(7) 0.0992(3) 0.0798(17) Uani 1 1 d .
H29 H 0.8285 0.3944 0.1028 0.096 Uiso 1 1 calc R
C30 C 0.6430(5) 0.3593(5) 0.1040(3) 0.0636(14) Uani 1 1 d .
H30 H 0.6212 0.4485 0.1108 0.076 Uiso 1 1 calc R
C31 C 0.5852(5) 0.1391(5) 0.0876(2) 0.0524(11) Uani 1 1 d .
C32 C 0.4881(5) 0.0447(4) 0.0777(2) 0.0539(12) Uani 1 1 d .
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'
Sn Sn -0.6537 1.4246 '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
S1 Sn1 S2 102.31(4) . .
S1 Sn1 S3 115.93(5) . 3_565
S2 Sn1 S3 115.55(4) . 3_565
S1 Sn1 S3 117.67(4) . .
S2 Sn1 S3 113.58(5) . .
S3 Sn1 S3 92.56(4) 3_565 .
S1 Sn1 Mn1 51.49(3) . .
S2 Sn1 Mn1 50.85(3) . .
S3 Sn1 Mn1 132.45(3) 3_565 .
S3 Sn1 Mn1 134.90(3) . .
Sn1 S1 Mn1 83.02(4) . .
Sn1 S2 Mn1 83.25(4) . .
Sn1 S3 Sn1 87.44(4) 3_565 .
N11 Mn1 N2 148.31(14) . .
N11 Mn1 N12 72.05(15) . .
N2 Mn1 N12 87.37(14) . .
N11 Mn1 N1 83.87(14) . .
N2 Mn1 N1 70.65(13) . .
N12 Mn1 N1 86.23(14) . .
N11 Mn1 S2 97.71(12) . .
N2 Mn1 S2 101.61(11) . .
N12 Mn1 S2 169.73(10) . .
N1 Mn1 S2 92.01(10) . .
N11 Mn1 S1 107.42(11) . .
N2 Mn1 S1 97.04(10) . .
N12 Mn1 S1 92.48(11) . .
N1 Mn1 S1 167.66(10) . .
S2 Mn1 S1 91.37(4) . .
N11 Mn1 Sn1 106.98(11) . .
N2 Mn1 Sn1 104.51(9) . .
N12 Mn1 Sn1 136.84(11) . .
N1 Mn1 Sn1 136.93(10) . .
S2 Mn1 Sn1 45.90(3) . .
S1 Mn1 Sn1 45.49(3) . .
C1 N1 C12 117.0(4) . .
C1 N1 Mn1 127.7(3) . .
C12 N1 Mn1 115.2(3) . .
C10 N2 C11 119.4(4) . .
C10 N2 Mn1 122.6(3) . .
C11 N2 Mn1 117.9(3) . .
N1 C1 C2 124.0(5) . .
C3 C2 C1 119.7(5) . .
C2 C3 C4 118.5(5) . .
C12 C4 C3 118.0(5) . .
C12 C4 C5 119.6(5) . .
C3 C4 C5 122.5(5) . .
C6 C5 C4 120.6(6) . .
C5 C6 C7 121.4(5) . .
C8 C7 C11 116.6(5) . .
C8 C7 C6 123.8(5) . .
C11 C7 C6 119.7(5) . .
C9 C8 C7 120.1(5) . .
C8 C9 C10 119.9(5) . .
N2 C10 C9 121.6(5) . .
N2 C11 C7 122.4(4) . .
N2 C11 C12 119.1(4) . .
C7 C11 C12 118.5(5) . .
N1 C12 C4 122.8(4) . .
N1 C12 C11 117.0(4) . .
C4 C12 C11 120.2(4) . .
C21 N11 C32 119.0(5) . .
C21 N11 Mn1 125.6(4) . .
C32 N11 Mn1 115.4(3) . .
C30 N12 C31 118.5(4) . .
C30 N12 Mn1 125.7(3) . .
C31 N12 Mn1 115.8(3) . .
N11 C21 C22 121.2(7) . .
C23 C22 C21 119.2(6) . .
C22 C23 C24 120.9(6) . .
C23 C24 C32 117.4(6) . .
C23 C24 C25 124.1(6) . .
C32 C24 C25 118.5(6) . .
C26 C25 C24 122.1(6) . .
C25 C26 C27 121.5(6) . .
C28 C27 C31 117.5(5) . .
C28 C27 C26 124.1(6) . .
C31 C27 C26 118.3(6) . .
C29 C28 C27 120.6(6) . .
C28 C29 C30 118.8(6) . .
N12 C30 C29 122.8(5) . .
N12 C31 C27 121.8(5) . .
N12 C31 C32 117.8(4) . .
C27 C31 C32 120.4(5) . .
N11 C32 C24 122.3(5) . .
N11 C32 C31 118.5(4) . .
C24 C32 C31 119.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3415(12) .
Sn1 S2 2.3566(12) .
Sn1 S3 2.4374(11) 3_565
Sn1 S3 2.4499(11) .
Sn1 Mn1 3.2590(7) .
S1 Mn1 2.5691(13) .
S2 Mn1 2.5451(14) .
S3 Sn1 2.4374(11) 3_565
Mn1 N11 2.287(4) .
Mn1 N2 2.300(4) .
Mn1 N12 2.305(4) .
Mn1 N1 2.382(4) .
N1 C1 1.321(6) .
N1 C12 1.364(6) .
N2 C10 1.318(6) .
N2 C11 1.337(6) .
C1 C2 1.380(8) .
C2 C3 1.361(8) .
C3 C4 1.412(8) .
C4 C12 1.392(7) .
C4 C5 1.430(8) .
C5 C6 1.344(9) .
C6 C7 1.420(8) .
C7 C8 1.403(8) .
C7 C11 1.414(7) .
C8 C9 1.340(9) .
C9 C10 1.402(8) .
C11 C12 1.438(6) .
N11 C21 1.328(7) .
N11 C32 1.366(7) .
N12 C30 1.331(6) .
N12 C31 1.346(6) .
C21 C22 1.432(9) .
C22 C23 1.361(10) .
C23 C24 1.379(9) .
C24 C32 1.418(7) .
C24 C25 1.440(10) .
C25 C26 1.318(10) .
C26 C27 1.433(8) .
C27 C28 1.391(9) .
C27 C31 1.421(8) .
C28 C29 1.348(9) .
C29 C30 1.401(8) .
C31 C32 1.422(7) .
