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#$Date: 2019-11-22 22:26:51 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231428 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/32/4003207.cif $
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#
# 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_4003207
loop_
_publ_author_name
'Ahmet, Ibbi Y.'
'Hill, Michael S.'
'Johnson, Andrew L.'
'Peter, Laurence M.'
_publ_section_title
;
 Polymorph-Selective Deposition of High Purity SnS Thin Films from a
 Single Source Precursor
;
_journal_issue                   22
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7680
_journal_paper_doi               10.1021/acs.chemmater.5b03220
_journal_volume                  27
_journal_year                    2015
_chemical_formula_moiety         'C22 H34 N6 S2 Sn2'
_chemical_formula_sum            'C22 H34 N6 S2 Sn2'
_chemical_formula_weight         684.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.0090(10)
_cell_angle_beta                 99.2320(10)
_cell_angle_gamma                94.8946(16)
_cell_formula_units_Z            1
_cell_length_a                   6.13510(10)
_cell_length_b                   8.9483(2)
_cell_length_c                   12.4437(3)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     670.31(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'SHELXL-2014 (Sheldrick, 2014)
;
_computing_structure_refinement
;
 SHELXL-2014/7 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '275 2.0 degree images with φ and 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  0.0426
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9999
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.654
_diffrn_reflns_theta_min         2.919
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.865
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0236P)²+5.5625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3256
_reflns_number_total             3385
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm5b03220_si_002.cif
_cod_data_source_block           K13ALJ31
_cod_database_code               4003207
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.580
_shelx_estimated_absorpt_t_max   0.749
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Sn1 Sn 0.70230(5) 0.01563(4) 0.11804(3) 0.01831(11) Uani 1 1 d . .
S11 S 0.4070(2) -0.02416(14) 0.24452(10) 0.0240(3) Uani 1 1 d . .
N1 N 0.4839(8) 0.1883(5) 0.4111(4) 0.0246(9) Uani 1 1 d . .
N2 N 0.4804(7) -0.1661(4) -0.0093(3) 0.0190(8) Uani 1 1 d . .
N12 N 0.7016(7) 0.2047(5) 0.2691(4) 0.0223(8) Uani 1 1 d . .
C1 C 0.6401(10) 0.2778(6) 0.4955(4) 0.0293(11) Uani 1 1 d . .
H1A H 0.7888 0.2825 0.4758 0.044 Uiso 1 1 calc R U
H1B H 0.6422 0.2314 0.5653 0.044 Uiso 1 1 calc R U
H1C H 0.5945 0.3797 0.5024 0.044 Uiso 1 1 calc R U
C2 C 0.2767(10) 0.1317(7) 0.4445(5) 0.0322(12) Uani 1 1 d . .
H2A H 0.1724 0.0879 0.3804 0.048 Uiso 1 1 calc R U
H2B H 0.2124 0.2146 0.4790 0.048 Uiso 1 1 calc R U
H2C H 0.3060 0.0546 0.4967 0.048 Uiso 1 1 calc R U
C3 C 0.3224(10) -0.2726(7) 0.0342(5) 0.0310(12) Uani 1 1 d . .
H3A H 0.2547 -0.3491 -0.0235 0.047 Uiso 1 1 calc R U
H3B H 0.2064 -0.2176 0.0592 0.047 Uiso 1 1 calc R U
H3C H 0.4019 -0.3212 0.0954 0.047 Uiso 1 1 calc R U
C4 C 0.6462(10) -0.2532(6) -0.0506(5) 0.0294(11) Uani 1 1 d . .
H4A H 0.7384 -0.2940 0.0106 0.044 Uiso 1 1 calc R U
H4B H 0.7400 -0.1876 -0.0888 0.044 Uiso 1 1 calc R U
H4C H 0.5704 -0.3360 -0.1013 0.044 Uiso 1 1 calc R U
C11 C 0.5415(8) 0.1418(5) 0.3152(4) 0.0202(9) Uani 1 1 d . .
C12 C 0.7838(8) 0.3574(6) 0.2801(4) 0.0208(9) Uani 1 1 d . .
C13 C 0.6536(9) 0.4740(6) 0.3021(4) 0.0234(10) Uani 1 1 d . .
H13 H 0.5115 0.4509 0.3214 0.028 Uiso 1 1 calc R U
C14 C 0.7337(10) 0.6236(6) 0.2954(4) 0.0276(11) Uani 1 1 d . .
H14 H 0.6440 0.7017 0.3090 0.033 Uiso 1 1 calc R U
C15 C 0.9412(10) 0.6594(6) 0.2692(5) 0.0316(12) Uani 1 1 d . .
H15 H 0.9940 0.7614 0.2645 0.038 Uiso 1 1 calc R U
C16 C 1.0729(10) 0.5443(7) 0.2498(5) 0.0326(12) Uani 1 1 d . .
H16 H 1.2168 0.5683 0.2329 0.039 Uiso 1 1 calc R U
C17 C 0.9941(9) 0.3942(6) 0.2552(4) 0.0257(10) Uani 1 1 d . .
H17 H 1.0848 0.3167 0.2417 0.031 Uiso 1 1 calc R U
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'
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
N2 Sn1 N2 80.15(15) 2_655 .
N2 Sn1 N12 87.63(15) 2_655 .
N2 Sn1 N12 145.24(14) . .
N2 Sn1 S11 96.53(11) 2_655 .
N2 Sn1 S11 87.71(10) . .
N12 Sn1 S11 61.35(11) . .
C11 S11 Sn1 84.40(17) . .
C11 N1 C1 121.9(5) . .
C11 N1 C2 122.3(5) . .
C1 N1 C2 115.0(4) . .
C4 N2 C3 108.0(4) . .
C4 N2 Sn1 119.0(3) . 2_655
C3 N2 Sn1 110.1(3) . 2_655
C4 N2 Sn1 103.0(3) . .
C3 N2 Sn1 117.0(3) . .
Sn1 N2 Sn1 99.85(15) 2_655 .
C11 N12 C12 126.8(4) . .
C11 N12 Sn1 100.2(3) . .
C12 N12 Sn1 129.3(3) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 H3A 109.5 . .
N2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N12 C11 N1 126.5(5) . .
N12 C11 S11 113.9(4) . .
N1 C11 S11 119.5(4) . .
C17 C12 N12 117.7(5) . .
C17 C12 C13 119.0(5) . .
N12 C12 C13 122.9(5) . .
C14 C13 C12 119.9(5) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.9(5) . .
C15 C14 H14 119.6 . .
C13 C14 H14 119.6 . .
C14 C15 C16 119.4(5) . .
C14 C15 H15 120.3 . .
C16 C15 H15 120.3 . .
C15 C16 C17 120.4(5) . .
C15 C16 H16 119.8 . .
C17 C16 H16 119.8 . .
C12 C17 C16 120.5(5) . .
C12 C17 H17 119.8 . .
C16 C17 H17 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 N2 2.205(4) 2_655
Sn1 N2 2.381(4) .
Sn1 N12 2.463(4) .
Sn1 S11 2.5980(13) .
S11 C11 1.755(5) .
N1 C11 1.353(6) .
N1 C1 1.457(7) .
N1 C2 1.459(7) .
N2 C4 1.473(7) .
N2 C3 1.484(7) .
N2 Sn1 2.205(4) 2_655
N12 C11 1.315(7) .
N12 C12 1.408(6) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C12 C17 1.391(7) .
C12 C13 1.408(7) .
C13 C14 1.398(7) .
C13 H13 0.9500 .
C14 C15 1.380(9) .
C14 H14 0.9500 .
C15 C16 1.396(9) .
C15 H15 0.9500 .
C16 C17 1.397(8) .
C16 H16 0.9500 .
C17 H17 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C12 N12 C11 N1 -28.5(8)
Sn1 N12 C11 N1 171.8(4)
C12 N12 C11 S11 155.3(4)
Sn1 N12 C11 S11 -4.4(4)
C1 N1 C11 N12 -24.0(8)
C2 N1 C11 N12 166.7(5)
C1 N1 C11 S11 152.0(4)
C2 N1 C11 S11 -17.2(7)
Sn1 S11 C11 N12 4.1(4)
Sn1 S11 C11 N1 -172.4(4)
C11 N12 C12 C17 159.8(5)
Sn1 N12 C12 C17 -46.4(6)
C11 N12 C12 C13 -28.0(8)
Sn1 N12 C12 C13 125.8(5)
C17 C12 C13 C14 1.9(8)
N12 C12 C13 C14 -170.2(5)
C12 C13 C14 C15 -1.1(8)
C13 C14 C15 C16 -0.4(9)
C14 C15 C16 C17 1.0(9)
N12 C12 C17 C16 171.2(5)
C13 C12 C17 C16 -1.3(8)
C15 C16 C17 C12 -0.1(9)
