#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:39:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179487 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/84/4338468.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_4338468
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         'Mn2C48H32N8, Sn2S6, C12H8N2, H2O'
_chemical_formula_sum            'C60 H42 Mn2 N10 O S6 Sn2'
_chemical_formula_weight         1458.66
_chemical_name_common            '[Mn(phen)2]2Sn2S6_phen_H2O'
_chemical_name_systematic
; 
 [Mn(C12H8N2)2]2Sn2S6_C12H8N2_H2O
;
_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-97
_cell_angle_alpha                113.200(4)
_cell_angle_beta                 90.908(5)
_cell_angle_gamma                110.974(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3203(7)
_cell_length_b                   12.1436(7)
_cell_length_c                   12.7586(7)
_cell_measurement_reflns_used    6406
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.77
_cell_volume                     1479.92(17)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13856
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.7856
_exptl_absorpt_correction_T_min  0.5192
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0284
_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)+(0.0456P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                4952
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500369m_si_005.cif
_cod_data_source_block           jh337
_cod_depositor_comments
'Adding full bibliography for 4338466--4338470.cif.'
_cod_original_cell_volume        1479.92(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338468
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.576269(19) 0.398596(18) 0.456150(15) 0.03202(6) Uani 1 1 d . . .
S1 S 0.79002(7) 0.44030(8) 0.43345(7) 0.04423(18) Uani 1 1 d . . .
S2 S 0.48443(7) 0.17238(7) 0.40179(6) 0.03773(16) Uani 1 1 d . . .
S3 S 0.53859(8) 0.52505(8) 0.64507(6) 0.04120(17) Uani 1 1 d . . .
Mn1 Mn 0.71356(4) 0.19508(4) 0.36420(3) 0.03310(10) Uani 1 1 d . . .
N1 N 0.6893(2) 0.1349(2) 0.16975(19) 0.0359(5) Uani 1 1 d . . .
N2 N 0.6365(2) -0.0328(2) 0.26942(18) 0.0333(5) Uani 1 1 d . . .
C1 C 0.7145(3) 0.2168(3) 0.1207(3) 0.0452(7) Uani 1 1 d . . .
H1 H 0.7395 0.3052 0.1683 0.054 Uiso 1 1 calc R . .
C2 C 0.7054(4) 0.1769(3) 0.0011(3) 0.0538(8) Uani 1 1 d . . .
H2 H 0.7241 0.2378 -0.0296 0.065 Uiso 1 1 calc R . .
C3 C 0.6689(3) 0.0485(3) -0.0695(3) 0.0530(8) Uani 1 1 d . . .
H3 H 0.6620 0.0205 -0.1493 0.064 Uiso 1 1 calc R . .
C4 C 0.6416(3) -0.0422(3) -0.0217(2) 0.0417(7) Uani 1 1 d . . .
C5 C 0.6011(4) -0.1790(3) -0.0905(3) 0.0539(8) Uani 1 1 d . . .
H5 H 0.5950 -0.2107 -0.1705 0.065 Uiso 1 1 calc R . .
C6 C 0.5716(4) -0.2625(3) -0.0414(3) 0.0556(9) Uani 1 1 d . . .
H6 H 0.5451 -0.3513 -0.0882 0.067 Uiso 1 1 calc R . .
C7 C 0.5801(3) -0.2178(3) 0.0814(3) 0.0450(7) Uani 1 1 d . . .
C8 C 0.5474(4) -0.3010(3) 0.1369(3) 0.0581(9) Uani 1 1 d . . .
H8 H 0.5176 -0.3909 0.0935 0.070 Uiso 1 1 calc R . .
C9 C 0.5593(4) -0.2496(3) 0.2553(3) 0.0539(8) Uani 1 1 d . . .
H9 H 0.5375 -0.3036 0.2933 0.065 Uiso 1 1 calc R . .
C10 C 0.6046(3) -0.1152(3) 0.3173(3) 0.0421(7) Uani 1 1 d . . .
H10 H 0.6129 -0.0812 0.3976 0.051 Uiso 1 1 calc R . .
C11 C 0.6234(3) -0.0831(3) 0.1523(2) 0.0327(5) Uani 1 1 d . . .
C12 C 0.6530(3) 0.0062(3) 0.0991(2) 0.0339(6) Uani 1 1 d . . .
N21 N 0.7824(2) 0.1791(2) 0.5226(2) 0.0418(5) Uani 1 1 d . . .
N22 N 0.9186(2) 0.1936(3) 0.3537(2) 0.0447(6) Uani 1 1 d . . .
C21 C 0.7142(4) 0.1726(3) 0.6053(3) 0.0536(8) Uani 1 1 d . . .
H21 H 0.6331 0.1744 0.5985 0.064 Uiso 1 1 calc R . .
C22 C 0.7609(5) 0.1632(4) 0.7022(3) 0.0707(11) Uani 1 1 d . . .
H22 H 0.7115 0.1594 0.7592 0.085 Uiso 1 1 calc R . .
C23 C 0.8787(5) 0.1597(4) 0.7123(3) 0.0770(13) Uani 1 1 d . . .
H23 H 0.9100 0.1527 0.7762 0.092 Uiso 1 1 calc R . .
C24 C 0.9530(4) 0.1666(4) 0.6274(3) 0.0624(10) Uani 1 1 d . . .
C25 C 1.0793(5) 0.1657(5) 0.6317(5) 0.0898(15) Uani 1 1 d . . .
H25 H 1.1151 0.1594 0.6941 0.108 Uiso 1 1 calc R . .
C26 C 1.1474(5) 0.1739(5) 0.5472(5) 0.0851(14) Uani 1 1 d . . .
H26 H 1.2293 0.1735 0.5527 0.102 Uiso 1 1 calc R . .
C27 C 1.0966(3) 0.1832(4) 0.4500(4) 0.0624(10) Uani 1 1 d . . .
C28 C 1.1637(4) 0.1919(4) 0.3608(5) 0.0800(13) Uani 1 1 d . . .
H28 H 1.2450 0.1897 0.3623 0.096 Uiso 1 1 calc R . .
C29 C 1.1104(4) 0.2033(5) 0.2730(5) 0.0793(13) Uani 1 1 d . . .
H29 H 1.1543 0.2105 0.2135 0.095 Uiso 1 1 calc R . .
C30 C 0.9881(3) 0.2041(4) 0.2732(4) 0.0619(9) Uani 1 1 d . . .
H30 H 0.9524 0.2127 0.2121 0.074 Uiso 1 1 calc R . .
C31 C 0.9729(3) 0.1842(3) 0.4422(3) 0.0453(7) Uani 1 1 d . . .
C32 C 0.9007(3) 0.1761(3) 0.5328(3) 0.0458(7) Uani 1 1 d . . .
N41 N 0.1429(4) 0.4851(4) 0.0502(3) 0.0748(10) Uani 0.50 1 d P . 1
C44' C 0.1429(4) 0.4851(4) 0.0502(3) 0.0748(10) Uani 0.50 1 d P . 2
C41 C 0.1957(5) 0.4823(5) 0.1461(5) 0.0917(14) Uani 1 1 d . . .
H41 H 0.2740 0.4736 0.1474 0.110 Uiso 1 1 calc R . 1
C42 C 0.1365(5) 0.4921(5) 0.2393(4) 0.0840(14) Uani 1 1 d . . .
H42 H 0.1731 0.4887 0.3031 0.101 Uiso 1 1 calc R . .
C43 C 0.0226(5) 0.5071(4) 0.2380(3) 0.0755(13) Uani 1 1 d . . .
H43 H -0.0172 0.5160 0.3023 0.091 Uiso 1 1 calc R . 1
C44 C -0.0344(4) 0.5092(3) 0.1426(3) 0.0647(9) Uani 0.50 1 d P . 1
N41' N -0.0344(4) 0.5092(3) 0.1426(3) 0.0647(9) Uani 0.50 1 d P . 2
C45 C 0.0282(4) 0.4985(4) 0.0504(3) 0.0573(9) Uani 1 1 d . . .
C46 C -0.1573(9) 0.5362(7) 0.1451(7) 0.068(2) Uani 0.50 1 d P . 1
H46 H -0.1946 0.5504 0.2111 0.082 Uiso 0.50 1 calc PR . 1
C47 C -0.2093(8) 0.5393(8) 0.0551(9) 0.076(2) Uani 0.50 1 d P . 1
H47 H -0.2835 0.5557 0.0549 0.091 Uiso 0.50 1 calc PR . 1
O1 O -0.2945(7) 0.5198(8) 0.1425(9) 0.133(3) Uani 0.50 1 d P A 2
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'
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 103.59(3) . .
S1 Sn1 S3 117.25(3) . .
S2 Sn1 S3 112.90(3) . .
S1 Sn1 S3 115.56(3) . 2_666
S2 Sn1 S3 114.80(3) . 2_666
S3 Sn1 S3 93.24(2) . 2_666
S1 Sn1 Mn1 51.33(2) . .
S2 Sn1 Mn1 52.284(19) . .
S3 Sn1 Mn1 134.66(2) . .
S3 Sn1 Mn1 132.055(18) 2_666 .
Sn1 S1 Mn1 82.80(3) . .
Sn1 S2 Mn1 81.57(2) . .
Sn1 S3 Sn1 86.76(2) . 2_666
N21 Mn1 N1 150.53(9) . .
N21 Mn1 N22 71.88(9) . .
N1 Mn1 N22 86.22(9) . .
N21 Mn1 N2 86.99(8) . .
N1 Mn1 N2 71.72(8) . .
N22 Mn1 N2 86.14(8) . .
N21 Mn1 S1 102.39(7) . .
N1 Mn1 S1 98.81(6) . .
N22 Mn1 S1 94.83(7) . .
N2 Mn1 S1 170.42(6) . .
N21 Mn1 S2 97.57(7) . .
N1 Mn1 S2 101.93(6) . .
N22 Mn1 S2 168.45(7) . .
N2 Mn1 S2 88.68(6) . .
S1 Mn1 S2 92.00(3) . .
N21 Mn1 Sn1 105.59(6) . .
N1 Mn1 Sn1 103.85(6) . .
N22 Mn1 Sn1 140.12(7) . .
N2 Mn1 Sn1 133.74(5) . .
S1 Mn1 Sn1 45.873(18) . .
S2 Mn1 Sn1 46.151(17) . .
C1 N1 C12 117.7(2) . .
C1 N1 Mn1 124.8(2) . .
C12 N1 Mn1 117.45(17) . .
C10 N2 C11 117.7(2) . .
C10 N2 Mn1 127.23(18) . .
C11 N2 Mn1 115.10(17) . .
N1 C1 C2 123.2(3) . .
C3 C2 C1 119.2(3) . .
C2 C3 C4 119.7(3) . .
C12 C4 C3 117.3(3) . .
C12 C4 C5 119.7(3) . .
C3 C4 C5 123.0(3) . .
C6 C5 C4 120.9(3) . .
C5 C6 C7 121.3(3) . .
C8 C7 C11 117.0(3) . .
C8 C7 C6 123.7(3) . .
C11 C7 C6 119.3(3) . .
C9 C8 C7 119.8(3) . .
C8 C9 C10 118.6(3) . .
N2 C10 C9 124.0(3) . .
N2 C11 C7 122.9(2) . .
N2 C11 C12 117.9(2) . .
C7 C11 C12 119.2(2) . .
N1 C12 C4 122.9(3) . .
N1 C12 C11 117.6(2) . .
C4 C12 C11 119.5(2) . .
C21 N21 C32 118.7(3) . .
C21 N21 Mn1 123.9(2) . .
C32 N21 Mn1 117.41(19) . .
C30 N22 C31 116.7(3) . .
C30 N22 Mn1 128.0(2) . .
C31 N22 Mn1 115.30(19) . .
N21 C21 C22 121.9(4) . .
C23 C22 C21 119.4(4) . .
C22 C23 C24 120.2(3) . .
C23 C24 C32 117.5(4) . .
C23 C24 C25 124.1(4) . .
C32 C24 C25 118.4(4) . .
C26 C25 C24 121.5(4) . .
C25 C26 C27 121.3(4) . .
C28 C27 C31 117.8(4) . .
C28 C27 C26 123.1(4) . .
C31 C27 C26 119.1(4) . .
C29 C28 C27 119.7(3) . .
C28 C29 C30 118.4(4) . .
N22 C30 C29 124.8(4) . .
N22 C31 C27 122.6(3) . .
N22 C31 C32 117.9(3) . .
C27 C31 C32 119.5(3) . .
N21 C32 C24 122.3(3) . .
N21 C32 C31 117.5(3) . .
C24 C32 C31 120.2(3) . .
C45 N41 C41 118.2(4) . .
C45 N41 C47 123.4(5) . 2_565
C41 N41 C47 118.2(5) . 2_565
C42 C41 N41 121.6(5) . .
C41 C42 C43 119.1(4) . .
C42 C43 C44 121.0(4) . .
C45 C44 C43 117.9(4) . .
C45 C44 C46 121.1(4) . .
C43 C44 C46 120.7(4) . .
N41 C45 C44 122.1(3) . .
N41 C45 C45 118.6(4) . 2_565
C44 C45 C45 119.3(4) . 2_565
C47 C46 C44 120.1(6) . .
C46 C47 N41 117.0(7) . 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3358(8) .
Sn1 S2 2.3537(8) .
Sn1 S3 2.4362(7) .
Sn1 S3 2.4437(7) 2_666
Sn1 Mn1 3.2285(5) .
S1 Mn1 2.5407(9) .
S2 Mn1 2.5818(8) .
S3 Sn1 2.4437(7) 2_666
Mn1 N21 2.257(2) .
Mn1 N1 2.274(2) .
Mn1 N22 2.333(2) .
Mn1 N2 2.342(2) .
N1 C1 1.325(4) .
N1 C12 1.357(3) .
N2 C10 1.317(3) .
N2 C11 1.355(3) .
C1 C2 1.397(4) .
C2 C3 1.354(5) .
C3 C4 1.404(4) .
C4 C12 1.402(4) .
C4 C5 1.426(4) .
C5 C6 1.340(5) .
C6 C7 1.431(4) .
C7 C8 1.402(4) .
C7 C11 1.407(4) .
C8 C9 1.372(5) .
C9 C10 1.386(5) .
C11 C12 1.441(4) .
N21 C21 1.327(4) .
N21 C32 1.358(4) .
N22 C30 1.322(4) .
N22 C31 1.340(4) .
C21 C22 1.398(5) .
C22 C23 1.355(6) .
C23 C24 1.392(6) .
C24 C32 1.398(4) .
C24 C25 1.435(6) .
C25 C26 1.350(7) .
C26 C27 1.420(6) .
C27 C28 1.395(6) .
C27 C31 1.408(4) .
C28 C29 1.341(7) .
C29 C30 1.389(5) .
C31 C32 1.441(4) .
N41 C45 1.364(5) .
N41 C41 1.370(6) .
N41 C47 1.529(9) 2_565
C41 C42 1.360(6) .
C42 C43 1.366(7) .
C43 C44 1.382(6) .
C44 C45 1.370(4) .
C44 C46 1.538(10) .
C45 C45 1.445(7) 2_565
C46 C47 1.301(13) .
C47 N41 1.529(9) 2_565
