#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/00/4300081.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_4300081
loop_
_publ_author_name
'Md. Munkir Hossain'
'Kazuko Matsumoto'
_publ_section_title
;
Pentasulfide S52- as the First Tridentate Chelating Ligand in
Ru(P(OE)3)3S5 (E = Me and Et)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              247
_journal_page_last               250
_journal_paper_doi               10.1021/ic990764j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C9 H27 O9 P3 S5 Ru '
_chemical_formula_sum            'C9 H27 O9 P3 Ru S5'
_chemical_formula_weight         633.60
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      144
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_audit_creation_date             'Mon May 31 16:52:41 1999'
_audit_creation_method           ' from TEXRAY.INF file'
_cell_angle_alpha                90.07(9)
_cell_angle_beta                 90.15(9)
_cell_angle_gamma                120.04(3)
_cell_formula_units_Z            3
_cell_length_a                   14.231(10)
_cell_length_b                   14.227(9)
_cell_length_c                   10.24(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      29.8
_cell_volume                     1795(2)
_computing_cell_refinement       ' Rigaku/AFC Diffractometer Control '
_computing_data_collection       ' Rigaku/AFC Diffractometer Control '
_computing_data_reduction        ' teXsan '
_computing_publication_material  ' teXsan '
_computing_structure_refinement  ' teXsan '
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device_type  ' Rigaku AFC7R '
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.07289
_diffrn_orient_matrix_UB_12      0.05937
_diffrn_orient_matrix_UB_13      -0.02860
_diffrn_orient_matrix_UB_21      0.02953
_diffrn_orient_matrix_UB_22      -0.05042
_diffrn_orient_matrix_UB_23      0.00822
_diffrn_orient_matrix_UB_31      -0.02011
_diffrn_orient_matrix_UB_32      -0.02295
_diffrn_orient_matrix_UB_33      -0.09300
_diffrn_radiation_detector       ' scintillation counter '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode '
_diffrn_radiation_type           ' Mo K/a '
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3064
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0.12
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   ' (Walker & Stuart, 1983 ) '
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    ' not measured '
_exptl_crystal_description       ' prismatic '
_exptl_crystal_F_000             966.00
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.01
_refine_diff_density_min         -1.27
_refine_ls_abs_structure_Flack   0.52(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   5.637
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1997
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.0030
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00002|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                1997
_reflns_number_total             2753
_reflns_threshold_expression     '>2.0 sigma (I)'
_cod_original_cell_volume        1794(2)
_cod_original_sg_symbol_H-M      ' P 31 '
_cod_original_formula_sum        'C9 H27 O9 P3 S5 Ru '
_cod_database_code               4300081
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,1/3+z
-x+y,-x,2/3+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
Ru Ru 0.33488(6) 0.33704(6) 0.00084(10) 0.0291(2) Uani 1.00 d . .
S(1) S 0.1826(2) 0.2272(3) -0.1476(3) 0.0676(9) Uani 1.00 d . .
S(2) S 0.2450(3) 0.2601(3) -0.3261(3) 0.110(1) Uani 1.00 d . .
S(3) S 0.3244(4) 0.4269(4) -0.3328(3) 0.123(1) Uani 1.00 d . .
S(4) S 0.4210(3) 0.4689(3) -0.1693(3) 0.0962(10) Uani 1.00 d . .
S(5) S 0.4592(3) 0.3374(3) -0.1695(3) 0.089(1) Uani 1.00 d . .
P(1) P 0.4829(2) 0.4319(2) 0.1266(2) 0.0403(7) Uani 1.00 d . .
P(2) P 0.2349(2) 0.3898(2) 0.1135(2) 0.0291(6) Uani 1.00 d . .
P(3) P 0.2790(2) 0.1850(2) 0.1158(3) 0.0394(6) Uani 1.00 d . .
O(1) O 0.5787(4) 0.5441(5) 0.0809(7) 0.055(2) Uani 1.00 d . .
O(2) O 0.4586(5) 0.4542(6) 0.2757(6) 0.062(2) Uani 1.00 d . .
O(3) O 0.5514(4) 0.3714(5) 0.1436(7) 0.054(2) Uani 1.00 d . .
O(4) O 0.2861(5) 0.5199(5) 0.1246(6) 0.049(2) Uani 1.00 d . .
O(5) O 0.2204(5) 0.3597(5) 0.2651(5) 0.047(2) Uani 1.00 d . .
O(6) O 0.1167(4) 0.3589(4) 0.0653(6) 0.044(2) Uani 1.00 d . .
O(7) O 0.3204(6) 0.2007(6) 0.2636(7) 0.070(2) Uani 1.00 d . .
O(8) O 0.1509(5) 0.1129(5) 0.1358(7) 0.053(2) Uani 1.00 d . .
O(9) O 0.3022(5) 0.0953(5) 0.0634(7) 0.060(2) Uani 1.00 d . .
C(1) C 0.5659(8) 0.6419(7) 0.073(1) 0.058(3) Uani 1.00 d . .
C(2) C 0.5284(9) 0.4815(10) 0.385(1) 0.086(4) Uani 1.00 d . .
C(3) C 0.6583(8) 0.4083(9) 0.116(1) 0.094(4) Uani 1.00 d . .
C(4) C 0.274(1) 0.5813(9) 0.024(1) 0.l09(5) Uani 1.00 d . .
C(5) C 0.1780(7) 0.4023(8) 0.3578(9) 0.054(3) Uani 1.00 d . .
C(6) C 0.0224(7) 0.2462(8) 0.070(1) 0.060(3) Uani 1.00 d . .
C(7) C 0.283(1) 0.140(1) 0.368(1) 0.113(5) Uani 1.00 d . .
C(8) C 0.081(1) 0.0019(9) 0.107(1) 0.109(5) Uani 1.00 d . .
C(9) C 0.4140(9) 0.1204(10) 0.055(1) 0.097(5) Uani 1.00 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
 International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
H H 0.000 0.000
;
International Tables for Crystallography 
(1992, Vol. C, Table 6.1.1.2) 
;
O O 0.011 0.006
;
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
S S 0.125 0.123
;
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
P P 0.102 0.094
;
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
Ru Ru -1.259 0.836
;
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 0 1
2 -1 0
0 2 -1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S(1) Ru S(4) 89.5(3) 1_555 1_555 1_555 yes
S(1) Ru S(5) 88.2(3) 1_555 1_555 1_555 yes
S(1) Ru P(1) 174.7(3) 1_555 1_555 1_555 yes
S(1) Ru P(2) 91.5(2) 1_555 1_555 1_555 yes
S(1) Ru P(3) 86.4(2) 1_555 1_555 1_555 yes
S(4) Ru S(5) 53.3(3) 1_555 1_555 1_555 yes
S(4) Ru P(1) 89.3(2) 1_555 1_555 1_555 yes
S(4) Ru P(2) 106.0(3) 1_555 1_555 1_555 yes
S(4) Ru P(3) 159.5(3) 1_555 1_555 1_555 yes
S(5) Ru P(1) 87.0(3) 1_555 1_555 1_555 yes
S(5) Ru P(2) 159.3(3) 1_555 1_555 1_555 yes
S(5) Ru P(3) 106.4(3) 1_555 1_555 1_555 yes
P(1) Ru P(2) 93.8(2) 1_555 1_555 1_555 yes
P(1) Ru P(3) 93.0(2) 1_555 1_555 1_555 yes
P(2) Ru P(3) 94.2(2) 1_555 1_555 1_555 yes
Ru S(1) S(2) 105.7(4) 1_555 1_555 1_555 yes
S(1) S(2) S(3) 103.2(5) 1_555 1_555 1_555 yes
S(2) S(3) S(4) 102.0(6) 1_555 1_555 1_555 yes
Ru S(4) S(3) 111.0(4) 1_555 1_555 1_555 yes
Ru S(4) S(5) 65.3(3) 1_555 1_555 1_555 yes
S(3) S(4) S(5) 99.6(6) 1_555 1_555 1_555 yes
Ru S(5) S(4) 61.4(2) 1_555 1_555 1_555 yes
Ru P(1) O(1) 121.0(7) 1_555 1_555 1_555 yes
Ru P(1) O(2) 115.1(6) 1_555 1_555 1_555 yes
Ru P(1) O(3) 112.2(6) 1_555 1_555 1_555 yes
O(1) P(1) O(2) 104.2(8) 1_555 1_555 1_555 yes
O(1) P(1) O(3) 97.4(8) 1_555 1_555 1_555 yes
O(2) P(1) O(3) 104.4(9) 1_555 1_555 1_555 yes
Ru P(2) O(4) 114.9(5) 1_555 1_555 1_555 yes
Ru P(2) O(5) 115.5(5) 1_555 1_555 1_555 yes
Ru P(2) O(6) 120.8(6) 1_555 1_555 1_555 yes
O(4) P(2) O(5) 99.5(8) 1_555 1_555 1_555 yes
O(4) P(2) O(6) 98.4(7) 1_555 1_555 1_555 yes
O(5) P(2) O(6) 104.4(8) 1_555 1_555 1_555 yes
Ru P(3) O(7) 116.0(7) 1_555 1_555 1_555 yes
Ru P(3) O(8) 115.5(6) 1_555 1_555 1_555 yes
Ru P(3) O(9) 119.4(7) 1_555 1_555 1_555 yes
O(7) P(3) O(8) 100.8(9) 1_555 1_555 1_555 yes
O(7) P(3) O(9) 103.0(9) 1_555 1_555 1_555 yes
O(8) P(3) O(9) 99.2(8) 1_555 1_555 1_555 yes
P(1) O(1) C(1) 121(1) 1_555 1_555 1_555 yes
P(1) O(2) C(2) 127(1) 1_555 1_555 1_555 yes
P(1) O(3) C(3) 129(1) 1_555 1_555 1_555 yes
P(2) O(4) C(4) 122(1) 1_555 1_555 1_555 yes
P(2) O(5) C(5) 124(1) 1_555 1_555 1_555 yes
P(2) O(6) C(6) 123(1) 1_555 1_555 1_555 yes
P(3) O(7) C(7) 132(2) 1_555 1_555 1_555 yes
P(3) O(8) C(8) 129(1) 1_555 1_555 1_555 yes
P(3) O(9) C(9) 118(1) 1_555 1_555 1_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru S(1) 2.456(6) 1_555 1_555 yes
Ru S(4) 2.403(7) 1_555 1_555 yes
Ru S(5) 2.485(6) 1_555 1_555 yes
Ru P(1) 2.248(6) 1_555 1_555 yes
Ru P(2) 2.236(6) 1_555 1_555 yes
Ru P(3) 2.233(6) 1_555 1_555 yes
S(1) S(2) 1.986(10) 1_555 1_555 yes
S(2) S(3) 2.06(1) 1_555 1_555 yes
S(3) S(4) 2.05(1) 1_555 1_555 yes
S(4) S(5) 2.19(1) 1_555 1_555 yes
P(1) O(1) 1.57(1) 1_555 1_555 yes
P(1) O(2) 1.63(1) 1_555 1_555 yes
P(1) O(3) 1.60(1) 1_555 1_555 yes
P(2) O(4) 1.62(1) 1_555 1_555 yes
P(2) O(5) 1.60(1) 1_555 1_555 yes
P(2) O(6) 1.59(1) 1_555 1_555 yes
P(3) O(7) 1.60(2) 1_555 1_555 yes
P(3) O(8) 1.60(1) 1_555 1_555 yes
P(3) O(9) 1.56(1) 1_555 1_555 yes
O(1) C(1) 1.49(2) 1_555 1_555 yes
O(2) C(2) 1.42(2) 1_555 1_555 yes
O(3) C(3) 1.37(2) 1_555 1_555 yes
O(4) C(4) 1.41(2) 1_555 1_555 yes
O(5) C(5) 1.41(2) 1_555 1_555 yes
O(6) C(6) 1.49(2) 1_555 1_555 yes
O(7) C(7) 1.31(2) 1_555 1_555 yes
O(8) C(8) 1.41(3) 1_555 1_555 yes
O(9) C(9) 1.45(3) 1_555 1_555 yes
