#------------------------------------------------------------------------------
#$Date: 2017-02-04 16:03:09 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191668 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/16/7041623.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_7041623
loop_
_publ_author_name
'Kühn, Michael'
'Lebedkin, Sergei'
'Weigend, Florian'
'Eichhöfer, Andreas'
_publ_section_title
;
 Optical properties of trinuclear metal chalcogenolate complexes - room
 temperature NIR fluorescence in [Cu2Ti(SPh)6(PPh3)2].
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1502
_journal_page_last               1509
_journal_paper_doi               10.1039/c6dt04287b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C72 H60 Ag2 P2 S6 Sn'
_chemical_formula_weight         1513.93
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-06-22 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.2373(19)
_cell_length_b                   13.2373(19)
_cell_length_c                   34.644(7)
_cell_measurement_reflns_used    20057
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.41
_cell_measurement_theta_min      1.75
_cell_volume                     5257.2(15)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            17659
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.011
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'Mo GeniX 3D HF'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.9206
_exptl_absorpt_correction_T_min  0.8299
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XRED32
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             2286
_exptl_crystal_recrystallization_method 'from reaction solution'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.753
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0298
_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)+(0.0243P)²+4.4530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3294
_reflns_number_total             4174
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04287b19.cif
_cod_data_source_block           r-3_sq
_cod_depositor_comments
'Adding full bibliography for 7041622--7041623.cif.'
_cod_original_cell_volume        5257.2(18)
_cod_database_code               7041623
_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. 
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_refinement_flags_occupancy
Sn1 Sn 0.0000 0.0000 0.0000 0.02460(6) Uani 1 6 d S T P
Ag1 Ag 0.0000 0.0000 0.09866(2) 0.04437(8) Uani 1 3 d S T P
S1 S 0.02928(4) -0.13199(3) 0.04740(2) 0.03131(9) Uani 1 1 d . . .
P1 P 0.0000 0.0000 0.16715(2) 0.03375(15) Uani 1 3 d S T P
C1 C 0.17266(16) -0.10870(15) 0.04293(5) 0.0346(3) Uani 1 1 d . . .
C2 C 0.26275(18) -0.02985(18) 0.06659(7) 0.0436(4) Uani 1 1 d . . .
H2 H 0.249(2) 0.015(2) 0.0857(8) 0.054(7) Uiso 1 1 d . . .
C3 C 0.3723(2) -0.0195(2) 0.06442(9) 0.0600(6) Uani 1 1 d . . .
H3 H 0.431(3) 0.031(3) 0.0793(9) 0.067(8) Uiso 1 1 d . . .
C4 C 0.3931(2) -0.0861(3) 0.03853(9) 0.0691(8) Uani 1 1 d . . .
H4 H 0.469(3) -0.080(3) 0.0376(9) 0.075(9) Uiso 1 1 d . . .
C5 C 0.3052(3) -0.1627(3) 0.01468(8) 0.0698(8) Uani 1 1 d . . .
H5 H 0.3202 -0.2075 -0.0034 0.084 Uiso 1 1 calc R U .
C6 C 0.1946(2) -0.1753(2) 0.01672(7) 0.0516(5) Uani 1 1 d . . .
H6 H 0.136(2) -0.225(2) 0.0008(7) 0.052(7) Uiso 1 1 d . . .
C7 C 0.01110(16) 0.13082(16) 0.18852(5) 0.0366(3) Uani 1 1 d . . .
C8 C 0.0738(2) 0.2345(2) 0.16869(7) 0.0548(6) Uani 1 1 d . . .
H8 H 0.109(2) 0.234(2) 0.1445(9) 0.070(8) Uiso 1 1 d . . .
C9 C 0.0855(3) 0.3371(2) 0.18385(9) 0.0683(7) Uani 1 1 d . . .
H9 H 0.129(3) 0.403(3) 0.1697(10) 0.079(9) Uiso 1 1 d . . .
C10 C 0.0342(2) 0.3362(2) 0.21824(8) 0.0563(6) Uani 1 1 d . . .
H10 H 0.045(2) 0.407(2) 0.2278(8) 0.063(8) Uiso 1 1 d . . .
C11 C -0.0272(2) 0.2337(2) 0.23859(8) 0.0537(5) Uani 1 1 d . . .
H11 H -0.059(2) 0.235(2) 0.2632(8) 0.060(7) Uiso 1 1 d . . .
C12 C -0.0389(2) 0.1313(2) 0.22375(7) 0.0472(5) Uani 1 1 d . . .
H12 H -0.084(2) 0.061(2) 0.2391(8) 0.064(8) Uiso 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'
Ag Ag -0.8971 1.1015 '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'
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 S1 180.000(14) 11 2
S1 Sn1 S1 83.400(17) 11 10
S1 Sn1 S1 96.600(17) 2 10
S1 Sn1 S1 83.400(18) 11 12
S1 Sn1 S1 96.600(18) 2 12
S1 Sn1 S1 83.400(17) 10 12
S1 Sn1 S1 96.600(18) 11 3
S1 Sn1 S1 83.400(18) 2 3
S1 Sn1 S1 96.600(17) 10 3
S1 Sn1 S1 180.000(19) 12 3
S1 Sn1 S1 96.600(17) 11 .
S1 Sn1 S1 83.400(18) 2 .
S1 Sn1 S1 180.0 10 .
S1 Sn1 S1 96.600(18) 12 .
S1 Sn1 S1 83.400(18) 3 .
P1 Ag1 S1 132.037(12) . .
P1 Ag1 S1 132.038(12) . 3
S1 Ag1 S1 80.062(18) . 3
P1 Ag1 S1 132.038(12) . 2
S1 Ag1 S1 80.062(18) . 2
S1 Ag1 S1 80.061(18) 3 2
C1 S1 Sn1 109.84(6) . .
C1 S1 Ag1 116.15(6) . .
Sn1 S1 Ag1 81.850(18) . .
C7 P1 C7 104.60(7) 3 2
C7 P1 C7 104.59(7) 3 .
C7 P1 C7 104.59(7) 2 .
C7 P1 Ag1 113.99(6) 3 .
C7 P1 Ag1 113.99(6) 2 .
C7 P1 Ag1 114.00(6) . .
C2 C1 C6 119.13(18) . .
C2 C1 S1 121.38(14) . .
C6 C1 S1 119.39(16) . .
C3 C2 C1 120.2(2) . .
C4 C3 C2 120.3(2) . .
C5 C4 C3 119.9(2) . .
C4 C5 C6 120.7(2) . .
C5 C6 C1 119.8(2) . .
C8 C7 C12 118.88(19) . .
C8 C7 P1 117.78(15) . .
C12 C7 P1 123.34(15) . .
C7 C8 C9 120.1(2) . .
C10 C9 C8 120.5(2) . .
C9 C10 C11 120.0(2) . .
C10 C11 C12 119.8(2) . .
C11 C12 C7 120.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.5644(5) 11
Sn1 S1 2.5644(5) 2
Sn1 S1 2.5644(5) 10
Sn1 S1 2.5644(5) 12
Sn1 S1 2.5644(5) 3
Sn1 S1 2.5644(5) .
Ag1 P1 2.3727(9) .
Ag1 S1 2.6522(5) .
Ag1 S1 2.6522(6) 3
Ag1 S1 2.6522(6) 2
S1 C1 1.7709(18) .
P1 C7 1.8204(19) 3
P1 C7 1.8205(19) 2
P1 C7 1.8205(19) .
C1 C2 1.392(3) .
C1 C6 1.393(3) .
C2 C3 1.388(3) .
C3 C4 1.379(4) .
C4 C5 1.372(4) .
C5 C6 1.391(3) .
C7 C8 1.380(3) .
C7 C12 1.390(3) .
C8 C9 1.390(3) .
C9 C10 1.368(4) .
C10 C11 1.377(4) .
C11 C12 1.384(3) .
