#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312624.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_4312624
loop_
_publ_author_name
'Kulbinder K. Banger'
'Michael H.-C. Jin'
'Jerry D. Harris'
'Philip E. Fanwick'
'Aloysius F. Hepp'
_publ_section_title
;
 A New Facile Route for the Preparation of Single-Source Precursors for
 Bulk, Thin-Film, and Nanocrystallite I-III-VI Semiconductors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7713
_journal_page_last               7715
_journal_paper_doi               10.1021/ic034802h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C40 H42 Ag In P2 S4'
_chemical_formula_weight         935.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 108.412(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6671(4)
_cell_length_b                   12.6092(4)
_cell_length_c                   21.6432(8)
_cell_measurement_temperature    150(2)
_cell_volume                     4056.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9646
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.363
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         9646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0299P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                5328
_reflns_number_total             9646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034802hsi20030710_073732.cif
_cod_data_source_block           xl
_cod_database_code               4312624
loop_
_publ_contact_author_name
_publ_contact_author_address
_publ_contact_author_email
_publ_contact_author_fax
_publ_contact_author_phone
'Kulbinder K. Banger'
;    NASA Glenn Research Center/Ohio Aerospace Institute
     Mailstop 302-1
     Clevaland
     OH 44135
     USA
;
KulbinderBanger@oai.org 1(216)6879298 1(216)6872004
'Aloysius F. Hepp'
;    NASA Glenn Research Center 
     Mailstop 302-1
     Clevaland
     OH 44135
     USA
;
Aloysius.F.Hepp@grc.nasa.goc 1(216)6106 1(2163835
'Phillip E. Fanwick'
;    Department of Chemistry
     Purdue University
     W. Lafayette
     IN 47907
     USA
;
fanwick@.xray.chem.purdue.edu 1(765)4940239 1(765)4944572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'-x, -y, -z'
'-x, y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.5000 0.44694(3) 0.2500 0.02492(11) Uani 1 2 d S . .
In2 In 0.0000 0.03306(3) 0.2500 0.02785(11) Uani 1 2 d S . .
Ag1 Ag 0.5000 0.16910(3) 0.2500 0.02577(11) Uani 1 2 d S . .
Ag2 Ag 0.0000 0.30776(3) 0.2500 0.02453(11) Uani 1 2 d S . .
S11 S 0.51639(8) 0.55483(8) 0.16155(6) 0.0374(3) Uani 1 1 d . . .
S12 S 0.37236(7) 0.32036(7) 0.21904(6) 0.0272(2) Uani 1 1 d . . .
S21 S -0.02599(8) -0.07913(8) 0.33378(6) 0.0415(3) Uani 1 1 d . . .
S22 S 0.12772(7) 0.15884(8) 0.28961(6) 0.0283(2) Uani 1 1 d . . .
P1 P 0.50628(7) 0.08309(8) 0.35323(5) 0.0229(2) Uani 1 1 d . . .
P2 P -0.00021(7) 0.39241(7) 0.35198(5) 0.0213(2) Uani 1 1 d . . .
C11 C 0.4332(3) 0.6582(3) 0.1570(2) 0.0402(11) Uani 1 1 d . . .
H11A H 0.3727 0.6276 0.1413 0.060 Uiso 1 1 calc R . .
H11B H 0.4390 0.7138 0.1270 0.060 Uiso 1 1 calc R . .
H11C H 0.4433 0.6888 0.2004 0.060 Uiso 1 1 calc R . .
C12 C 0.3319(3) 0.3332(3) 0.1303(2) 0.0440(12) Uani 1 1 d . . .
H12A H 0.2886 0.3916 0.1179 0.066 Uiso 1 1 calc R . .
H12B H 0.3027 0.2670 0.1109 0.066 Uiso 1 1 calc R . .
H12C H 0.3828 0.3479 0.1145 0.066 Uiso 1 1 calc R . .
C21 C 0.0497(3) -0.1881(3) 0.3333(3) 0.0459(13) Uani 1 1 d . . .
H21A H 0.0715 -0.1808 0.2958 0.069 Uiso 1 1 calc R . .
H21B H 0.0175 -0.2555 0.3304 0.069 Uiso 1 1 calc R . .
H21C H 0.1008 -0.1867 0.3736 0.069 Uiso 1 1 calc R . .
C22 C 0.1899(3) 0.1350(3) 0.2319(2) 0.0364(11) Uani 1 1 d . . .
H22A H 0.2155 0.0635 0.2385 0.055 Uiso 1 1 calc R . .
H22B H 0.2384 0.1872 0.2391 0.055 Uiso 1 1 calc R . .
H22C H 0.1489 0.1417 0.1873 0.055 Uiso 1 1 calc R . .
C114 C 0.7624(3) -0.1111(3) 0.4499(2) 0.0378(11) Uani 1 1 d . . .
H114 H 0.8159 -0.1502 0.4696 0.045 Uiso 1 1 calc R . .
C112 C 0.6812(3) 0.0153(3) 0.3705(2) 0.0335(10) Uani 1 1 d . . .
H112 H 0.6790 0.0621 0.3356 0.040 Uiso 1 1 calc R . .
C113 C 0.7574(3) -0.0435(4) 0.3991(2) 0.0410(12) Uani 1 1 d . . .
H113 H 0.8074 -0.0374 0.3834 0.049 Uiso 1 1 calc R . .
C111 C 0.6074(2) 0.0062(3) 0.39287(19) 0.0240(9) Uani 1 1 d . . .
C115 C 0.6898(3) -0.1219(3) 0.4724(2) 0.0349(10) Uani 1 1 d . . .
H115 H 0.6926 -0.1695 0.5070 0.042 Uiso 1 1 calc R . .
C116 C 0.6122(3) -0.0629(3) 0.4440(2) 0.0303(10) Uani 1 1 d . . .
H116 H 0.5622 -0.0699 0.4596 0.036 Uiso 1 1 calc R . .
C121 C 0.4954(3) 0.1792(3) 0.4130(2) 0.0243(9) Uani 1 1 d . . .
C122 C 0.5521(3) 0.1866(3) 0.4768(2) 0.0294(9) Uani 1 1 d . . .
H122 H 0.5992 0.1363 0.4928 0.035 Uiso 1 1 calc R . .
C123 C 0.5406(3) 0.2670(3) 0.5176(2) 0.0368(11) Uani 1 1 d . . .
H123 H 0.5795 0.2712 0.5612 0.044 Uiso 1 1 calc R . .
C124 C 0.4728(3) 0.3406(3) 0.4947(2) 0.0419(12) Uani 1 1 d . . .
H124 H 0.4653 0.3958 0.5224 0.050 Uiso 1 1 calc R . .
C125 C 0.4161(3) 0.3343(3) 0.4317(2) 0.0404(12) Uani 1 1 d . . .
H125 H 0.3693 0.3849 0.4162 0.048 Uiso 1 1 calc R . .
C126 C 0.4265(3) 0.2548(3) 0.3905(2) 0.0311(10) Uani 1 1 d . . .
H126 H 0.3870 0.2513 0.3471 0.037 Uiso 1 1 calc R . .
C131 C 0.4164(2) -0.0129(3) 0.34653(19) 0.0232(9) Uani 1 1 d . . .
C132 C 0.3470(3) 0.0018(3) 0.3721(2) 0.0326(10) Uani 1 1 d . . .
H132 H 0.3454 0.0636 0.3968 0.039 Uiso 1 1 calc R . .
C133 C 0.2794(3) -0.0741(3) 0.3616(2) 0.0412(12) Uani 1 1 d . . .
H133 H 0.2314 -0.0634 0.3790 0.049 Uiso 1 1 calc R . .
C134 C 0.2812(3) -0.1630(3) 0.3268(3) 0.0430(12) Uani 1 1 d . . .
H134 H 0.2344 -0.2138 0.3198 0.052 Uiso 1 1 calc R . .
C135 C 0.3509(3) -0.1801(3) 0.3016(3) 0.0429(12) Uani 1 1 d . . .
H135 H 0.3528 -0.2431 0.2780 0.051 Uiso 1 1 calc R . .
C136 C 0.4174(3) -0.1048(3) 0.3113(2) 0.0360(11) Uani 1 1 d . . .
H136 H 0.4649 -0.1159 0.2935 0.043 Uiso 1 1 calc R . .
C211 C 0.1089(2) 0.4456(3) 0.39979(19) 0.0229(9) Uani 1 1 d . . .
C212 C 0.1534(3) 0.5124(3) 0.3693(2) 0.0312(10) Uani 1 1 d . . .
H212 H 0.1270 0.5280 0.3243 0.037 Uiso 1 1 calc R . .
C213 C 0.2356(3) 0.5566(3) 0.4034(2) 0.0405(12) Uani 1 1 d . . .
H213 H 0.2649 0.6028 0.3819 0.049 Uiso 1 1 calc R . .
C214 C 0.2753(3) 0.5338(3) 0.4689(2) 0.0379(11) Uani 1 1 d . . .
H214 H 0.3316 0.5643 0.4925 0.045 Uiso 1 1 calc R . .
C215 C 0.2317(3) 0.4657(3) 0.4993(2) 0.0354(10) Uani 1 1 d . . .
H215 H 0.2589 0.4484 0.5439 0.043 Uiso 1 1 calc R . .
C216 C 0.1485(2) 0.4227(3) 0.46525(19) 0.0270(9) Uani 1 1 d . . .
H216 H 0.1187 0.3774 0.4869 0.032 Uiso 1 1 calc R . .
C221 C -0.0309(2) 0.3033(3) 0.40790(19) 0.0216(8) Uani 1 1 d . . .
C222 C 0.0032(3) 0.1999(3) 0.4148(2) 0.0286(9) Uani 1 1 d . . .
H222 H 0.0431 0.1787 0.3919 0.034 Uiso 1 1 calc R . .
C223 C -0.0209(3) 0.1287(3) 0.4548(2) 0.0355(10) Uani 1 1 d . . .
H223 H 0.0024 0.0585 0.4591 0.043 Uiso 1 1 calc R . .
C224 C -0.0789(3) 0.1586(3) 0.4888(2) 0.0331(10) Uani 1 1 d . . .
H224 H -0.0957 0.1090 0.5160 0.040 Uiso 1 1 calc R . .
C225 C -0.1119(2) 0.2608(3) 0.48277(19) 0.0282(9) Uani 1 1 d . . .
H225 H -0.1512 0.2818 0.5062 0.034 Uiso 1 1 calc R . .
C226 C -0.0881(2) 0.3330(3) 0.4428(2) 0.0262(9) Uani 1 1 d . . .
H226 H -0.1110 0.4033 0.4392 0.031 Uiso 1 1 calc R . .
C231 C -0.0768(2) 0.5036(3) 0.34550(19) 0.0210(8) Uani 1 1 d . . .
C232 C -0.0541(3) 0.5915(3) 0.38593(19) 0.0255(9) Uani 1 1 d . . .
H232 H 0.0033 0.5956 0.4181 0.031 Uiso 1 1 calc R . .
C233 C -0.1159(3) 0.6739(3) 0.3793(2) 0.0310(10) Uani 1 1 d . . .
H233 H -0.0998 0.7347 0.4064 0.037 Uiso 1 1 calc R . .
C234 C -0.1997(3) 0.6677(3) 0.3339(2) 0.0347(11) Uani 1 1 d . . .
H234 H -0.2414 0.7241 0.3296 0.042 Uiso 1 1 calc R . .
C235 C -0.2233(3) 0.5793(3) 0.2944(2) 0.0359(11) Uani 1 1 d . . .
H235 H -0.2817 0.5744 0.2634 0.043 Uiso 1 1 calc R . .
C236 C -0.1622(3) 0.4979(3) 0.2998(2) 0.0296(9) Uani 1 1 d . . .
H236 H -0.1787 0.4377 0.2722 0.036 Uiso 1 1 calc R . .
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'
P P 0.1023 0.0942 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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
_geom_angle_publ_flag
S11 In1 S11 111.83(6) 4_656 . ?
S11 In1 S12 107.26(3) 4_656 . ?
S11 In1 S12 115.13(4) . . ?
S11 In1 S12 115.13(4) 4_656 4_656 ?
S11 In1 S12 107.26(3) . 4_656 ?
S12 In1 S12 99.87(5) . 4_656 ?
S21 In2 S21 108.91(5) 4_556 . ?
S21 In2 S22 108.80(3) 4_556 . ?
S21 In2 S22 114.84(4) . . ?
S21 In2 S22 114.85(4) 4_556 4_556 ?
S21 In2 S22 108.80(3) . 4_556 ?
S22 In2 S22 100.64(5) . 4_556 ?
P1 Ag1 P1 127.63(5) 4_656 . ?
P1 Ag1 S12 105.85(3) 4_656 . ?
P1 Ag1 S12 110.64(3) . . ?
P1 Ag1 S12 110.64(3) 4_656 4_656 ?
P1 Ag1 S12 105.85(3) . 4_656 ?
S12 Ag1 S12 89.71(4) . 4_656 ?
P2 Ag2 P2 128.40(5) . 4_556 ?
P2 Ag2 S22 112.32(3) . 4_556 ?
P2 Ag2 S22 103.31(3) 4_556 4_556 ?
P2 Ag2 S22 103.30(3) . . ?
P2 Ag2 S22 112.32(3) 4_556 . ?
S22 Ag2 S22 91.03(5) 4_556 . ?
C11 S11 In1 101.02(14) . . ?
C12 S12 In1 102.06(15) . . ?
C12 S12 Ag1 107.93(14) . . ?
In1 S12 Ag1 85.21(3) . . ?
C21 S21 In2 99.95(14) . . ?
C22 S22 In2 101.74(14) . . ?
C22 S22 Ag2 113.59(15) . . ?
In2 S22 Ag2 84.16(3) . . ?
C121 P1 C111 106.40(19) . . ?
C121 P1 C131 104.77(17) . . ?
C111 P1 C131 102.62(17) . . ?
C121 P1 Ag1 111.49(12) . . ?
C111 P1 Ag1 116.19(12) . . ?
C131 P1 Ag1 114.30(13) . . ?
C231 P2 C211 103.73(17) . . ?
C231 P2 C221 102.71(16) . . ?
C211 P2 C221 104.26(18) . . ?
C231 P2 Ag2 116.98(13) . . ?
C211 P2 Ag2 113.79(11) . . ?
C221 P2 Ag2 113.86(12) . . ?
C113 C114 C115 119.9(4) . . ?
C113 C112 C111 119.8(4) . . ?
C114 C113 C112 121.1(4) . . ?
C112 C111 C116 119.1(4) . . ?
C112 C111 P1 119.1(3) . . ?
C116 C111 P1 121.8(3) . . ?
C114 C115 C116 119.7(4) . . ?
C115 C116 C111 120.4(3) . . ?
C122 C121 C126 118.5(4) . . ?
C122 C121 P1 125.3(3) . . ?
C126 C121 P1 116.1(3) . . ?
C121 C122 C123 120.5(4) . . ?
C124 C123 C122 120.1(4) . . ?
C125 C124 C123 120.0(4) . . ?
C124 C125 C126 120.6(4) . . ?
C125 C126 C121 120.1(4) . . ?
C132 C131 C136 118.6(4) . . ?
C132 C131 P1 124.4(3) . . ?
C136 C131 P1 117.0(3) . . ?
C131 C132 C133 119.9(4) . . ?
C134 C133 C132 120.7(4) . . ?
C133 C134 C135 120.4(4) . . ?
C136 C135 C134 119.1(4) . . ?
C135 C136 C131 121.4(4) . . ?
C216 C211 C212 118.9(4) . . ?
C216 C211 P2 122.8(3) . . ?
C212 C211 P2 118.4(3) . . ?
C213 C212 C211 120.9(4) . . ?
C212 C213 C214 120.3(4) . . ?
C213 C214 C215 119.0(4) . . ?
C214 C215 C216 120.7(4) . . ?
C211 C216 C215 120.3(4) . . ?
C226 C221 C222 118.8(3) . . ?
C226 C221 P2 122.9(3) . . ?
C222 C221 P2 118.3(3) . . ?
C223 C222 C221 120.2(4) . . ?
C222 C223 C224 120.6(4) . . ?
C225 C224 C223 119.5(4) . . ?
C224 C225 C226 120.4(4) . . ?
C225 C226 C221 120.5(3) . . ?
C232 C231 C236 119.1(3) . . ?
C232 C231 P2 122.4(3) . . ?
C236 C231 P2 118.5(3) . . ?
C231 C232 C233 119.9(4) . . ?
C234 C233 C232 120.5(4) . . ?
C233 C234 C235 119.9(4) . . ?
C236 C235 C234 120.2(4) . . ?
C235 C236 C231 120.4(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 S11 2.4273(11) 4_656 ?
In1 S11 2.4273(11) . ?
In1 S12 2.4797(10) . ?
In1 S12 2.4797(10) 4_656 ?
In2 S21 2.4333(11) 4_556 ?
In2 S21 2.4334(11) . ?
In2 S22 2.4841(11) . ?
In2 S22 2.4841(11) 4_556 ?
Ag1 P1 2.4574(10) 4_656 ?
Ag1 P1 2.4574(10) . ?
Ag1 S12 2.6906(10) . ?
Ag1 S12 2.6907(10) 4_656 ?
Ag2 P2 2.4527(10) . ?
Ag2 P2 2.4527(10) 4_556 ?
Ag2 S22 2.6797(10) 4_556 ?
Ag2 S22 2.6797(10) . ?
S11 C11 1.824(4) . ?
S12 C12 1.830(5) . ?
S21 C21 1.816(4) . ?
S22 C22 1.834(4) . ?
P1 C121 1.819(4) . ?
P1 C111 1.824(4) . ?
P1 C131 1.827(4) . ?
P2 C231 1.822(4) . ?
P2 C211 1.823(4) . ?
P2 C221 1.824(4) . ?
C114 C113 1.374(6) . ?
C114 C115 1.378(5) . ?
C112 C113 1.375(6) . ?
C112 C111 1.392(5) . ?
C111 C116 1.392(5) . ?
C115 C116 1.391(5) . ?
C121 C122 1.390(6) . ?
C121 C126 1.407(5) . ?
C122 C123 1.393(5) . ?
C123 C124 1.380(6) . ?
C124 C125 1.375(7) . ?
C125 C126 1.384(5) . ?
C131 C132 1.379(5) . ?
C131 C136 1.390(5) . ?
C132 C133 1.392(5) . ?
C133 C134 1.355(6) . ?
C134 C135 1.383(6) . ?
C135 C136 1.376(5) . ?
C211 C216 1.386(5) . ?
C211 C212 1.387(5) . ?
C212 C213 1.384(6) . ?
C213 C214 1.385(6) . ?
C214 C215 1.387(6) . ?
C215 C216 1.388(5) . ?
C221 C226 1.394(5) . ?
C221 C222 1.398(5) . ?
C222 C223 1.380(5) . ?
C223 C224 1.390(5) . ?
C224 C225 1.379(5) . ?
C225 C226 1.385(5) . ?
C231 C232 1.387(5) . ?
C231 C236 1.392(5) . ?
C232 C233 1.396(5) . ?
C233 C234 1.371(6) . ?
C234 C235 1.383(6) . ?
C235 C236 1.382(5) . ?
