#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:39:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179487 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/84/4338466.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_4338466
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, Sn2S8, Mn2C24H16N4, H2O'
_chemical_formula_sum            'C72 H50 Mn4 N12 O S8 Sn2'
_chemical_formula_weight         1812.86
_chemical_name_common            '[Mn(phen)2]2[SnS4]2[Mn(phen)]2_H2O'
_chemical_name_systematic
; 
 [Mn(C12H8N2)2]2[SnS4]2[Mn(12H8N2)]2_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                103.381(3)
_cell_angle_beta                 108.390(3)
_cell_angle_gamma                101.636(4)
_cell_formula_units_Z            1
_cell_length_a                   10.8703(5)
_cell_length_b                   12.5183(6)
_cell_length_c                   14.9644(6)
_cell_measurement_reflns_used    7768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.51
_cell_volume                     1794.71(16)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18641
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_T_max  0.8413
_exptl_absorpt_correction_T_min  0.7010
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0412
_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)+(0.0497P)²+1.6665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                6507
_reflns_number_total             7768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500369m_si_006.cif
_cod_data_source_block           jh336
_cod_depositor_comments
'Adding full bibliography for 4338466--4338470.cif.'
_cod_original_cell_volume        1794.71(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338466
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 0.39047(3) 0.34218(2) 0.756310(19) 0.03089(8) Uani 1 1 d . . .
S1 S 0.15776(10) 0.25154(9) 0.65560(8) 0.0375(2) Uani 1 1 d . . .
S2 S 0.48746(10) 0.35797(9) 0.63698(8) 0.0379(2) Uani 1 1 d . . .
S3 S 0.47099(10) 0.53517(8) 0.87679(7) 0.0346(2) Uani 1 1 d . . .
S4 S 0.48507(12) 0.24571(9) 0.86824(8) 0.0408(2) Uani 1 1 d . . .
Mn1 Mn 0.24496(6) 0.25719(5) 0.51663(4) 0.03183(14) Uani 1 1 d . . .
N1 N 0.1840(3) 0.4053(3) 0.4766(3) 0.0356(7) Uani 1 1 d . . .
N2 N 0.0279(3) 0.1830(3) 0.3860(3) 0.0354(7) Uani 1 1 d . . .
C1 C 0.2628(5) 0.5126(4) 0.5183(3) 0.0431(10) Uani 1 1 d . . .
H1 H 0.3484 0.5277 0.5666 0.052 Uiso 1 1 calc R . .
C2 C 0.2236(5) 0.6046(4) 0.4931(4) 0.0521(12) Uani 1 1 d . . .
H2 H 0.2824 0.6791 0.5237 0.063 Uiso 1 1 calc R . .
C3 C 0.0981(5) 0.5838(4) 0.4232(4) 0.0504(11) Uani 1 1 d . . .
H3 H 0.0703 0.6443 0.4059 0.061 Uiso 1 1 calc R . .
C4 C 0.0111(4) 0.4715(4) 0.3774(3) 0.0388(9) Uani 1 1 d . . .
C5 C -0.1227(5) 0.4423(4) 0.3033(4) 0.0476(11) Uani 1 1 d . . .
H5 H -0.1555 0.5004 0.2851 0.057 Uiso 1 1 calc R . .
C6 C -0.2010(5) 0.3333(5) 0.2600(4) 0.0500(11) Uani 1 1 d . . .
H6 H -0.2880 0.3169 0.2131 0.060 Uiso 1 1 calc R . .
C7 C -0.1536(4) 0.2407(4) 0.2844(3) 0.0409(9) Uani 1 1 d . . .
C8 C -0.2300(5) 0.1243(4) 0.2388(4) 0.0512(11) Uani 1 1 d . . .
H8 H -0.3166 0.1038 0.1902 0.061 Uiso 1 1 calc R . .
C9 C -0.1775(5) 0.0412(4) 0.2657(4) 0.0497(11) Uani 1 1 d . . .
H9 H -0.2268 -0.0361 0.2352 0.060 Uiso 1 1 calc R . .
C10 C -0.0476(5) 0.0749(4) 0.3402(3) 0.0424(9) Uani 1 1 d . . .
H10 H -0.0126 0.0178 0.3584 0.051 Uiso 1 1 calc R . .
C11 C -0.0243(4) 0.2665(3) 0.3580(3) 0.0346(8) Uani 1 1 d . . .
C12 C 0.0600(4) 0.3833(3) 0.4055(3) 0.0327(8) Uani 1 1 d . . .
N21 N 0.7994(4) 0.3709(4) 1.0388(3) 0.0512(10) Uani 1 1 d . . .
N22 N 0.8046(4) 0.5905(4) 1.0554(3) 0.0509(10) Uani 1 1 d . . .
C21 C 0.7961(6) 0.2631(5) 1.0303(4) 0.0605(14) Uani 1 1 d . . .
H21 H 0.7128 0.2064 0.9965 0.073 Uiso 1 1 calc R . .
C22 C 0.9115(7) 0.2297(7) 1.0694(5) 0.0767(18) Uani 1 1 d . . .
H22 H 0.9044 0.1526 1.0624 0.092 Uiso 1 1 calc R . .
C23 C 1.0342(6) 0.3113(7) 1.1180(5) 0.0767(19) Uani 1 1 d . . .
H23 H 1.1119 0.2903 1.1443 0.092 Uiso 1 1 calc R . .
C24 C 1.0435(5) 0.4261(6) 1.1284(4) 0.0651(16) Uani 1 1 d . . .
C25 C 1.1670(6) 0.5163(8) 1.1773(5) 0.080(2) Uani 1 1 d . . .
H25 H 1.2477 0.4993 1.2035 0.096 Uiso 1 1 calc R . .
C26 C 1.1695(6) 0.6254(8) 1.1864(5) 0.083(2) Uani 1 1 d . . .
H26 H 1.2523 0.6828 1.2189 0.100 Uiso 1 1 calc R . .
C27 C 1.0484(5) 0.6570(6) 1.1476(4) 0.0679(16) Uani 1 1 d . . .
C28 C 1.0453(6) 0.7693(6) 1.1548(5) 0.080(2) Uani 1 1 d . . .
H28 H 1.1256 0.8296 1.1865 0.096 Uiso 1 1 calc R . .
C29 C 0.9259(7) 0.7914(6) 1.1160(5) 0.0788(19) Uani 1 1 d . . .
H29 H 0.9235 0.8666 1.1232 0.095 Uiso 1 1 calc R . .
C30 C 0.8045(6) 0.6980(5) 1.0640(5) 0.0625(14) Uani 1 1 d . . .
H30 H 0.7231 0.7129 1.0354 0.075 Uiso 1 1 calc R . .
C31 C 0.9236(5) 0.5685(5) 1.0967(3) 0.0537(13) Uani 1 1 d . . .
C32 C 0.9219(5) 0.4532(5) 1.0882(3) 0.0520(12) Uani 1 1 d . . .
Mn2 Mn 0.61638(6) 0.43926(5) 0.98956(5) 0.03490(14) Uani 1 1 d . . .
N41 N 0.3249(3) 0.2362(3) 0.3855(3) 0.0353(7) Uani 1 1 d . . .
N42 N 0.2664(4) 0.0792(3) 0.4752(3) 0.0373(7) Uani 1 1 d . . .
C41 C 0.3559(5) 0.3135(4) 0.3426(4) 0.0448(10) Uani 1 1 d . . .
H41 H 0.3402 0.3839 0.3623 0.054 Uiso 1 1 calc R . .
C42 C 0.4103(6) 0.2960(5) 0.2703(4) 0.0571(13) Uani 1 1 d . . .
H42 H 0.4281 0.3524 0.2413 0.068 Uiso 1 1 calc R . .
C43 C 0.4372(6) 0.1945(5) 0.2425(5) 0.0656(15) Uani 1 1 d . . .
H43 H 0.4734 0.1811 0.1938 0.079 Uiso 1 1 calc R . .
C44 C 0.4102(5) 0.1095(4) 0.2872(4) 0.0472(11) Uani 1 1 d . . .
C45 C 0.4397(6) 0.0029(5) 0.2664(4) 0.0592(14) Uani 1 1 d . . .
H45 H 0.4764 -0.0148 0.2185 0.071 Uiso 1 1 calc R . .
C46 C 0.4160(5) -0.0727(4) 0.3140(4) 0.0529(12) Uani 1 1 d . . .
H46 H 0.4392 -0.1405 0.2999 0.063 Uiso 1 1 calc R . .
C47 C 0.3560(4) -0.0511(4) 0.3860(3) 0.0402(9) Uani 1 1 d . . .
C48 C 0.3254(5) -0.1281(4) 0.4351(4) 0.0517(11) Uani 1 1 d . . .
H48 H 0.3460 -0.1973 0.4230 0.062 Uiso 1 1 calc R . .
C49 C 0.2650(6) -0.1018(4) 0.5011(4) 0.0585(14) Uani 1 1 d . . .
H49 H 0.2415 -0.1535 0.5329 0.070 Uiso 1 1 calc R . .
C50 C 0.2394(6) 0.0040(4) 0.5198(4) 0.0496(11) Uani 1 1 d . . .
H50 H 0.2010 0.0225 0.5665 0.060 Uiso 1 1 calc R . .
C51 C 0.3236(4) 0.0534(3) 0.4080(3) 0.0337(8) Uani 1 1 d . . .
C52 C 0.3533(4) 0.1359(3) 0.3595(3) 0.0364(8) Uani 1 1 d . . .
O1 O 0.4383(15) 0.0880(13) 0.0087(8) 0.140(5) Uani 0.50 1 d P . .
H1O1 H 0.4476 0.1489 0.0489 0.210 Uiso 0.25 1 d PR A 1
H2O1 H 0.3551 0.0662 -0.0144 0.210 Uiso 0.25 1 d PR A 1
H3O1 H 0.4461 0.1523 0.0029 0.210 Uiso 0.25 1 d PR A 2
H4O1 H 0.5145 0.0822 0.0337 0.210 Uiso 0.25 1 d PR 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 102.17(4) . .
S1 Sn1 S4 113.99(4) . .
S2 Sn1 S4 116.12(4) . .
S1 Sn1 S3 121.99(4) . .
S2 Sn1 S3 105.60(4) . .
S4 Sn1 S3 97.55(4) . .
S1 Sn1 Mn1 51.38(3) . .
S2 Sn1 Mn1 50.81(3) . .
S4 Sn1 Mn1 131.47(3) . .
S3 Sn1 Mn1 130.31(3) . .
Sn1 S1 Mn1 82.19(3) . .
Sn1 S2 Mn1 82.67(3) . .
Sn1 S3 Mn2 116.60(4) . 2_667
Sn1 S3 Mn2 82.44(3) . .
Mn2 S3 Mn2 80.14(3) 2_667 .
Sn1 S4 Mn2 86.62(4) . .
N1 Mn1 N42 151.70(13) . .
N1 Mn1 N41 86.63(12) . .
N42 Mn1 N41 71.72(12) . .
N1 Mn1 N2 72.11(12) . .
N42 Mn1 N2 87.28(12) . .
N41 Mn1 N2 83.85(12) . .
N1 Mn1 S2 100.48(10) . .
N42 Mn1 S2 97.00(10) . .
N41 Mn1 S2 88.43(9) . .
N2 Mn1 S2 169.55(9) . .
N1 Mn1 S1 100.59(9) . .
N42 Mn1 S1 100.55(9) . .
N41 Mn1 S1 172.26(9) . .
N2 Mn1 S1 95.64(9) . .
S2 Mn1 S1 92.95(4) . .
N1 Mn1 Sn1 106.17(9) . .
N42 Mn1 Sn1 102.01(9) . .
N41 Mn1 Sn1 134.29(9) . .
N2 Mn1 Sn1 141.83(8) . .
S2 Mn1 Sn1 46.52(2) . .
S1 Mn1 Sn1 46.44(3) . .
C1 N1 C12 118.5(3) . .
C1 N1 Mn1 123.3(3) . .
C12 N1 Mn1 118.2(3) . .
C10 N2 C11 117.6(4) . .
C10 N2 Mn1 128.8(3) . .
C11 N2 Mn1 113.6(3) . .
N1 C1 C2 122.9(4) . .
C3 C2 C1 119.1(4) . .
C2 C3 C4 119.9(4) . .
C3 C4 C12 117.3(4) . .
C3 C4 C5 123.3(4) . .
C12 C4 C5 119.3(4) . .
C6 C5 C4 121.2(4) . .
C5 C6 C7 121.3(4) . .
C11 C7 C8 117.5(4) . .
C11 C7 C6 118.9(4) . .
C8 C7 C6 123.6(4) . .
C9 C8 C7 120.1(4) . .
C8 C9 C10 118.6(4) . .
N2 C10 C9 123.7(4) . .
N2 C11 C7 122.5(4) . .
N2 C11 C12 117.4(4) . .
C7 C11 C12 120.1(4) . .
N1 C12 C4 122.3(4) . .
N1 C12 C11 118.6(3) . .
C4 C12 C11 119.1(4) . .
C21 N21 C32 117.8(4) . .
C21 N21 Mn2 126.9(4) . .
C32 N21 Mn2 115.1(3) . .
C30 N22 C31 119.3(5) . .
C30 N22 Mn2 124.2(4) . .
C31 N22 Mn2 116.1(4) . .
N21 C21 C22 123.3(6) . .
C23 C22 C21 119.1(7) . .
C22 C23 C24 120.0(5) . .
C23 C24 C32 117.6(6) . .
C23 C24 C25 123.6(6) . .
C32 C24 C25 118.8(7) . .
C26 C25 C24 121.0(6) . .
C25 C26 C27 122.1(6) . .
C28 C27 C31 117.3(6) . .
C28 C27 C26 124.5(6) . .
C31 C27 C26 118.3(7) . .
C29 C28 C27 120.5(6) . .
C28 C29 C30 119.2(7) . .
N22 C30 C29 121.6(6) . .
N22 C31 C27 122.1(6) . .
N22 C31 C32 118.7(4) . .
C27 C31 C32 119.2(5) . .
N21 C32 C24 122.2(6) . .
N21 C32 C31 117.1(4) . .
C24 C32 C31 120.6(5) . .
N22 Mn2 N21 72.54(16) . .
N22 Mn2 S3 101.30(10) . 2_667
N21 Mn2 S3 107.27(11) . 2_667
N22 Mn2 S4 149.38(10) . .
N21 Mn2 S4 88.53(12) . .
S3 Mn2 S4 107.31(4) 2_667 .
N22 Mn2 S3 94.60(12) . .
N21 Mn2 S3 151.69(11) . .
S3 Mn2 S3 99.86(3) 2_667 .
S4 Mn2 S3 91.09(4) . .
C41 N41 C52 117.7(4) . .
C41 N41 Mn1 128.1(3) . .
C52 N41 Mn1 113.9(3) . .
C50 N42 C51 118.5(3) . .
C50 N42 Mn1 123.5(3) . .
C51 N42 Mn1 117.6(3) . .
N41 C41 C42 124.1(4) . .
C43 C42 C41 118.7(5) . .
C42 C43 C44 120.2(5) . .
C43 C44 C52 116.4(4) . .
C43 C44 C45 124.6(4) . .
C52 C44 C45 119.0(4) . .
C46 C45 C44 121.8(4) . .
C45 C46 C47 121.3(4) . .
C48 C47 C51 117.8(4) . .
C48 C47 C46 123.6(4) . .
C51 C47 C46 118.6(4) . .
C49 C48 C47 119.7(4) . .
C48 C49 C50 118.7(5) . .
N42 C50 C49 123.6(4) . .
N42 C51 C47 121.6(4) . .
N42 C51 C52 118.3(3) . .
C47 C51 C52 120.0(4) . .
N41 C52 C44 122.9(4) . .
N41 C52 C51 117.9(3) . .
C44 C52 C51 119.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3670(11) .
Sn1 S2 2.3678(10) .
Sn1 S4 2.3816(11) .
Sn1 S3 2.4471(10) .
Sn1 Mn1 3.2363(7) .
S1 Mn1 2.5521(12) .
S2 Mn1 2.5289(12) .
S3 Mn2 2.4555(11) 2_667
S3 Mn2 2.6090(12) .
S4 Mn2 2.4775(13) .
Mn1 N1 2.234(3) .
Mn1 N42 2.251(3) .
Mn1 N41 2.368(3) .
Mn1 N2 2.370(4) .
N1 C1 1.319(5) .
N1 C12 1.354(5) .
N2 C10 1.321(6) .
N2 C11 1.371(5) .
C1 C2 1.396(6) .
C2 C3 1.362(7) .
C3 C4 1.397(7) .
C4 C12 1.410(5) .
C4 C5 1.435(7) .
C5 C6 1.335(7) .
C6 C7 1.435(6) .
C7 C11 1.403(6) .
C7 C8 1.405(7) .
C8 C9 1.363(7) .
C9 C10 1.401(7) .
C11 C12 1.432(6) .
N21 C21 1.319(7) .
N21 C32 1.361(7) .
N21 Mn2 2.299(4) .
N22 C30 1.322(7) .
N22 C31 1.360(6) .
N22 Mn2 2.246(4) .
C21 C22 1.397(7) .
C22 C23 1.359(10) .
C23 C24 1.388(10) .
C24 C32 1.413(7) .
C24 C25 1.414(10) .
C25 C26 1.335(11) .
C26 C27 1.435(9) .
C27 C28 1.393(10) .
C27 C31 1.414(7) .
C28 C29 1.357(10) .
C29 C30 1.422(8) .
C31 C32 1.416(8) .
Mn2 S3 2.4555(11) 2_667
N41 C41 1.324(5) .
N41 C52 1.353(5) .
N42 C50 1.310(5) .
N42 C51 1.352(5) .
C41 C42 1.383(7) .
C42 C43 1.362(8) .
C43 C44 1.412(7) .
C44 C52 1.415(6) .
C44 C45 1.423(7) .
C45 C46 1.341(8) .
C46 C47 1.428(6) .
C47 C48 1.390(7) .
C47 C51 1.415(5) .
C48 C49 1.363(7) .
C49 C50 1.392(6) .
C51 C52 1.434(6) .
