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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100760.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_1100760
loop_
_publ_author_name
'Sergey M. Dibrov'
'Bin Deng'
'Donald E. Ellis'
'James A. Ibers'
_publ_contact_author_name        'James A. Ibers'
_publ_section_title
;

Synthesis and Structural Characterization of Some Selenoruthenates and

Telluroruthenates

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3441
_journal_page_last               3448
_journal_paper_doi               10.1021/ic0483646
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C46 H40 P2 Ru2 Se4'
_chemical_formula_weight         1172.70
_chemical_name_systematic
;

?

;
_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                93.561(3)
_cell_angle_beta                 93.604(3)
_cell_angle_gamma                109.951(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5419(14)
_cell_length_b                   11.8807(17)
_cell_length_c                   11.9229(18)
_cell_measurement_reflns_used    3844
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.72
_cell_volume                     1263.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker 1000-CCD'
_diffrn_measurement_method       'omega 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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13958
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    3.570
_exptl_absorpt_correction_T_max  0.93407
_exptl_absorpt_correction_T_min  0.74289
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0443
_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)+(0.0680P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                3436
_reflns_number_total             5146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0483646si20041124_025321_2.cif
_cod_data_source_block           Ru2Se4
_cod_database_code               1100760
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
Ru1 Ru 0.07912(5) 0.15215(4) 0.13978(4) 0.02444(15) Uani 1 1 d . . .
Se1 Se 0.19293(7) 0.16348(5) -0.03697(5) 0.02568(17) Uani 1 1 d . . .
Se2 Se 0.00785(7) -0.05847(5) 0.16843(5) 0.02640(17) Uani 1 1 d . . .
P1 P 0.30542(18) 0.18522(14) 0.23675(13) 0.0244(4) Uani 1 1 d . . .
C1 C 0.4616(7) 0.3160(6) 0.2026(5) 0.0292(14) Uani 1 1 d . . .
C2 C 0.4353(9) 0.4143(6) 0.1650(6) 0.050(2) Uani 1 1 d . . .
H2 H 0.3373 0.4134 0.1562 0.060 Uiso 1 1 calc R . .
C3 C 0.5504(9) 0.5148(6) 0.1400(6) 0.051(2) Uani 1 1 d . . .
H3 H 0.5301 0.5807 0.1149 0.061 Uiso 1 1 calc R . .
C4 C 0.6930(10) 0.5163(7) 0.1523(8) 0.064(3) Uani 1 1 d . . .
H4 H 0.7703 0.5816 0.1314 0.077 Uiso 1 1 calc R . .
C5 C 0.7243(11) 0.4232(8) 0.1950(14) 0.123(6) Uani 1 1 d . . .
H5 H 0.8231 0.4272 0.2082 0.148 Uiso 1 1 calc R . .
C6 C 0.6083(10) 0.3222(8) 0.2188(12) 0.095(4) Uani 1 1 d . . .
H6 H 0.6298 0.2577 0.2462 0.114 Uiso 1 1 calc R . .
C7 C 0.3898(6) 0.0680(5) 0.2364(5) 0.0260(13) Uani 1 1 d . . .
C8 C 0.3781(7) -0.0035(6) 0.1371(5) 0.0304(14) Uani 1 1 d . . .
H8 H 0.3248 0.0075 0.0732 0.036 Uiso 1 1 calc R . .
C9 C 0.4444(7) -0.0916(6) 0.1311(6) 0.0351(16) Uani 1 1 d . . .
H9 H 0.4377 -0.1374 0.0634 0.042 Uiso 1 1 calc R . .
C10 C 0.5195(8) -0.1097(6) 0.2261(6) 0.0383(17) Uani 1 1 d . . .
H10 H 0.5614 -0.1698 0.2236 0.046 Uiso 1 1 calc R . .
C11 C 0.5333(8) -0.0388(7) 0.3260(6) 0.0419(18) Uani 1 1 d . . .
H11 H 0.5871 -0.0501 0.3894 0.050 Uiso 1 1 calc R . .
C12 C 0.4676(7) 0.0487(6) 0.3318(5) 0.0340(15) Uani 1 1 d . . .
H12 H 0.4753 0.0945 0.3995 0.041 Uiso 1 1 calc R . .
C13 C 0.2927(7) 0.2159(6) 0.3881(5) 0.0288(14) Uani 1 1 d . . .
C14 C 0.2014(8) 0.1257(6) 0.4439(5) 0.0362(17) Uani 1 1 d . . .
H14 H 0.1527 0.0506 0.4051 0.043 Uiso 1 1 calc R . .
C15 C 0.1796(7) 0.1431(7) 0.5564(6) 0.0391(17) Uani 1 1 d . . .
H15 H 0.1209 0.0794 0.5935 0.047 Uiso 1 1 calc R . .
C16 C 0.2442(9) 0.2532(7) 0.6116(6) 0.0470(19) Uani 1 1 d . . .
H16 H 0.2308 0.2658 0.6874 0.056 Uiso 1 1 calc R . .
C17 C 0.3285(12) 0.3452(8) 0.5566(7) 0.077(3) Uani 1 1 d . . .
H17 H 0.3686 0.4218 0.5941 0.093 Uiso 1 1 calc R . .
C18 C 0.3562(9) 0.3276(7) 0.4454(6) 0.053(2) Uani 1 1 d . . .
H18 H 0.4175 0.3912 0.4097 0.064 Uiso 1 1 calc R . .
C19 C 0.0423(8) 0.3064(6) 0.2335(6) 0.0384(17) Uani 1 1 d . . .
H19 H 0.1166 0.3594 0.2847 0.046 Uiso 1 1 calc R . .
C20 C -0.0678(9) 0.2001(7) 0.2580(6) 0.046(2) Uani 1 1 d . . .
H20 H -0.0794 0.1702 0.3284 0.055 Uiso 1 1 calc R . .
C21 C -0.1574(8) 0.1467(6) 0.1577(7) 0.0418(18) Uani 1 1 d . . .
H21 H -0.2396 0.0757 0.1508 0.050 Uiso 1 1 calc R . .
C22 C -0.1031(8) 0.2178(6) 0.0695(6) 0.0355(16) Uani 1 1 d . . .
H22 H -0.1405 0.2020 -0.0059 0.043 Uiso 1 1 calc R . .
C23 C 0.0205(8) 0.3187(6) 0.1178(6) 0.0386(17) Uani 1 1 d . . .
H23 H 0.0773 0.3821 0.0794 0.046 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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
C19 Ru1 C20 36.6(3) . . ?
C19 Ru1 C23 36.5(2) . . ?
C20 Ru1 C23 60.7(3) . . ?
C19 Ru1 C21 60.8(3) . . ?
C20 Ru1 C21 36.5(3) . . ?
C23 Ru1 C21 60.2(3) . . ?
C19 Ru1 C22 61.3(2) . . ?
C20 Ru1 C22 61.0(2) . . ?
C23 Ru1 C22 36.6(2) . . ?
C21 Ru1 C22 36.1(3) . . ?
C19 Ru1 P1 93.78(18) . . ?
C20 Ru1 P1 108.0(2) . . ?
C23 Ru1 P1 114.98(19) . . ?
C21 Ru1 P1 144.0(2) . . ?
C22 Ru1 P1 151.52(18) . . ?
C19 Ru1 Se2 132.8(2) . . ?
C20 Ru1 Se2 98.1(2) . . ?
C23 Ru1 Se2 150.98(19) . . ?
C21 Ru1 Se2 90.85(18) . . ?
C22 Ru1 Se2 117.22(18) . . ?
P1 Ru1 Se2 89.45(5) . . ?
C19 Ru1 Se1 124.4(2) . . ?
C20 Ru1 Se1 152.37(19) . . ?
C23 Ru1 Se1 93.06(19) . . ?
C21 Ru1 Se1 124.6(2) . . ?
C22 Ru1 Se1 93.03(18) . . ?
P1 Ru1 Se1 90.36(5) . . ?
Se2 Ru1 Se1 102.67(3) . . ?
Se2 Se1 Ru1 103.40(3) 2 . ?
Se1 Se2 Ru1 107.83(3) 2 . ?
C7 P1 C1 101.9(3) . . ?
C7 P1 C13 102.1(3) . . ?
C1 P1 C13 103.8(3) . . ?
C7 P1 Ru1 120.9(2) . . ?
C1 P1 Ru1 116.3(2) . . ?
C13 P1 Ru1 109.6(2) . . ?
C2 C1 C6 117.6(7) . . ?
C2 C1 P1 120.3(5) . . ?
C6 C1 P1 122.1(6) . . ?
C1 C2 C3 121.7(8) . . ?
C4 C3 C2 119.3(8) . . ?
C3 C4 C5 120.6(8) . . ?
C4 C5 C6 119.6(9) . . ?
C1 C6 C5 120.9(9) . . ?
C8 C7 C12 118.5(6) . . ?
C8 C7 P1 119.1(5) . . ?
C12 C7 P1 122.5(5) . . ?
C7 C8 C9 121.5(6) . . ?
C10 C9 C8 119.1(6) . . ?
C9 C10 C11 120.4(6) . . ?
C12 C11 C10 120.5(6) . . ?
C11 C12 C7 120.1(6) . . ?
C14 C13 C18 117.8(6) . . ?
C14 C13 P1 118.2(5) . . ?
C18 C13 P1 123.6(5) . . ?
C13 C14 C15 121.9(6) . . ?
C16 C15 C14 119.3(7) . . ?
C15 C16 C17 119.8(7) . . ?
C16 C17 C18 121.3(7) . . ?
C13 C18 C17 119.8(7) . . ?
C20 C19 C23 107.9(6) . . ?
C20 C19 Ru1 71.7(4) . . ?
C23 C19 Ru1 72.9(4) . . ?
C19 C20 C21 108.0(6) . . ?
C19 C20 Ru1 71.6(4) . . ?
C21 C20 Ru1 73.0(4) . . ?
C22 C21 C20 109.0(6) . . ?
C22 C21 Ru1 72.4(4) . . ?
C20 C21 Ru1 70.6(4) . . ?
C21 C22 C23 106.7(6) . . ?
C21 C22 Ru1 71.6(4) . . ?
C23 C22 Ru1 71.2(4) . . ?
C19 C23 C22 108.4(6) . . ?
C19 C23 Ru1 70.6(4) . . ?
C22 C23 Ru1 72.2(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
Ru1 C19 2.228(6) . ?
Ru1 C20 2.229(7) . ?
Ru1 C23 2.258(6) . ?
Ru1 C21 2.260(7) . ?
Ru1 C22 2.271(6) . ?
Ru1 P1 2.2813(17) . ?
Ru1 Se2 2.4114(8) . ?
Ru1 Se1 2.4211(8) . ?
Se1 Se2 2.3307(9) 2 ?
Se2 Se1 2.3307(9) 2 ?
P1 C7 1.831(6) . ?
P1 C1 1.837(6) . ?
P1 C13 1.838(6) . ?
C1 C2 1.371(9) . ?
C1 C6 1.377(11) . ?
C2 C3 1.383(10) . ?
C3 C4 1.353(11) . ?
C4 C5 1.360(13) . ?
C5 C6 1.386(12) . ?
C7 C8 1.389(9) . ?
C7 C12 1.392(8) . ?
C8 C9 1.396(9) . ?
C9 C10 1.370(9) . ?
C10 C11 1.387(10) . ?
C11 C12 1.386(9) . ?
C13 C14 1.369(9) . ?
C13 C18 1.372(9) . ?
C14 C15 1.384(9) . ?
C15 C16 1.348(10) . ?
C16 C17 1.353(11) . ?
C17 C18 1.385(11) . ?
C19 C20 1.401(10) . ?
C19 C23 1.406(9) . ?
C20 C21 1.405(11) . ?
C21 C22 1.402(10) . ?
C22 C23 1.423(9) . ?
