#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/00/01/8000167.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_8000167
loop_
_publ_author_name
'Arashiba, Kazuya'
'Tanabe, Yoshiaki'
'Ishii, Youichi'
_publ_section_title
;
 Synthesis and Reactivities of Sulfido-bridged Ir--W and Ir--Re
 Heterodinuclear Complexes with Imido Ligands
;
_journal_issue                   5
_journal_name_full               'Chemistry Letters'
_journal_page_first              622
_journal_paper_doi               10.1246/cl.2007.622
_journal_volume                  36
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C13 H24 Ir O2 P S2 W '
_chemical_formula_sum            'C13 H24 Ir O2 P S2 W'
_chemical_formula_weight         683.50
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.4702(12)
_cell_length_b                   12.985(2)
_cell_length_c                   16.275(3)
_cell_measurement_reflns_used    5540
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1790.0(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13699
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    14.197
_exptl_absorpt_correction_T_max  0.119
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.30
_refine_diff_density_min         -1.55
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1745 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.018(9)
_refine_ls_extinction_coef       4.8(14)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3664
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.0161
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.6700σ(Fo²)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0254
_reflns_number_gt                3664
_reflns_number_total             4065
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            36-622sup1.cif
_cod_data_source_block           '__Cp*Ir(PMe3)(m-S)2W(O)2'
_cod_original_formula_sum        'C13 H24 Ir O2 P S2 W '
_cod_database_code               8000167
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,-Z
3 -X,1/2+Y,1/2-Z
4 1/2-X,-Y,1/2+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
Ir(1) Ir 0.40976(3) 0.04095(2) 0.655670(10) 0.00711(5) Uani 1.00 1 d .
W(1) W 0.14109(3) -0.09286(2) 0.67997(2) 0.01214(6) Uani 1.00 1 d .
S(1) S 0.1723(2) 0.02336(12) 0.57625(11) 0.0140(4) Uani 1.00 1 d .
S(2) S 0.3846(2) -0.11110(12) 0.73781(11) 0.0158(4) Uani 1.00 1 d .
P(1) P 0.5283(2) -0.05520(14) 0.55513(12) 0.0136(4) Uani 1.00 1 d .
O(1) O 0.0035(6) -0.0479(4) 0.7505(3) 0.0221(14) Uani 1.00 1 d .
O(2) O 0.0798(6) -0.2113(3) 0.6409(3) 0.0212(13) Uani 1.00 1 d .
C(1) C 0.3339(7) 0.2003(4) 0.6963(4) 0.0098(13) Uiso 1.00 1 d .
C(2) C 0.4630(8) 0.2044(5) 0.6373(4) 0.0154(18) Uani 1.00 1 d .
C(3) C 0.5986(8) 0.1569(4) 0.6743(4) 0.0141(16) Uani 1.00 1 d .
C(4) C 0.5511(7) 0.1171(4) 0.7532(4) 0.0106(16) Uani 1.00 1 d .
C(5) C 0.3878(7) 0.1452(4) 0.7670(4) 0.0102(13) Uiso 1.00 1 d .
C(6) C 0.1754(8) 0.2486(5) 0.6843(5) 0.0202(19) Uani 1.00 1 d .
C(7) C 0.4643(9) 0.2653(5) 0.5599(4) 0.023(2) Uani 1.00 1 d .
C(8) C 0.7623(8) 0.1603(5) 0.6435(5) 0.022(2) Uani 1.00 1 d .
C(9) C 0.6573(8) 0.0711(5) 0.8152(4) 0.0194(18) Uani 1.00 1 d .
C(10) C 0.2956(8) 0.1232(5) 0.8430(4) 0.0189(17) Uani 1.00 1 d .
C(11) C 0.5394(9) 0.0125(6) 0.4572(4) 0.025(2) Uani 1.00 1 d .
C(12) C 0.7299(8) -0.0932(6) 0.5772(5) 0.028(2) Uani 1.00 1 d .
C(13) C 0.4350(8) -0.1768(5) 0.5289(4) 0.021(2) Uani 1.00 1 d .
H(1) H 0.1633 0.2814 0.6325 0.024 Uiso 1.00 1 c R
H(2) H 0.1587 0.2973 0.7269 0.024 Uiso 1.00 1 c R
H(3) H 0.1007 0.1944 0.6891 0.024 Uiso 1.00 1 c R
H(4) H 0.5693 0.2648 0.5393 0.028 Uiso 1.00 1 c R
H(5) H 0.4346 0.3339 0.5730 0.028 Uiso 1.00 1 c R
H(6) H 0.3947 0.2386 0.5193 0.028 Uiso 1.00 1 c R
H(7) H 0.8271 0.1276 0.6834 0.026 Uiso 1.00 1 c R
H(8) H 0.7992 0.2284 0.6343 0.026 Uiso 1.00 1 c R
H(9) H 0.7663 0.1225 0.5936 0.026 Uiso 1.00 1 c R
H(10) H 0.5971 0.0574 0.8632 0.023 Uiso 1.00 1 c R
H(11) H 0.7389 0.1187 0.8279 0.023 Uiso 1.00 1 c R
H(12) H 0.7025 0.0089 0.7955 0.023 Uiso 1.00 1 c R
H(13) H 0.1895 0.1459 0.8373 0.023 Uiso 1.00 1 c R
H(14) H 0.3435 0.1577 0.8881 0.023 Uiso 1.00 1 c R
H(15) H 0.2971 0.0510 0.8526 0.023 Uiso 1.00 1 c R
H(16) H 0.4470 -0.0014 0.4261 0.030 Uiso 1.00 1 c R
H(17) H 0.6296 -0.0098 0.4275 0.030 Uiso 1.00 1 c R
H(18) H 0.5468 0.0844 0.4672 0.030 Uiso 1.00 1 c R
H(19) H 0.8021 -0.0430 0.5576 0.034 Uiso 1.00 1 c R
H(20) H 0.7500 -0.1572 0.5509 0.034 Uiso 1.00 1 c R
H(21) H 0.7424 -0.1010 0.6349 0.034 Uiso 1.00 1 c R
H(22) H 0.4762 -0.2298 0.5630 0.026 Uiso 1.00 1 c R
H(23) H 0.4532 -0.1938 0.4729 0.026 Uiso 1.00 1 c R
H(24) H 0.3248 -0.1701 0.5382 0.026 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ir Ir -1.444 7.990
;
International Tables for Crystallography
(1992, 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
W(1) Ir(1) S(1) 49.99(4)
W(1) Ir(1) S(2) 50.03(4)
W(1) Ir(1) P(1) 96.62(4)
W(1) Ir(1) C(1) 106.61(16)
W(1) Ir(1) C(2) 139.77(18)
W(1) Ir(1) C(3) 163.20(17)
W(1) Ir(1) C(4) 126.49(17)
W(1) Ir(1) C(5) 100.64(16)
S(1) Ir(1) S(2) 98.48(5)
S(1) Ir(1) P(1) 86.04(6)
S(1) Ir(1) C(1) 90.36(17)
S(1) Ir(1) C(2) 101.02(19)
S(1) Ir(1) C(3) 137.92(17)
S(1) Ir(1) C(4) 151.47(16)
S(1) Ir(1) C(5) 114.68(16)
S(2) Ir(1) P(1) 89.34(6)
S(2) Ir(1) C(1) 124.42(16)
S(2) Ir(1) C(2) 153.4(2)
S(2) Ir(1) C(3) 123.22(17)
S(2) Ir(1) C(4) 90.94(17)
S(2) Ir(1) C(5) 92.23(16)
P(1) Ir(1) C(1) 146.18(17)
P(1) Ir(1) C(2) 109.89(19)
P(1) Ir(1) C(3) 98.73(17)
P(1) Ir(1) C(4) 121.13(17)
P(1) Ir(1) C(5) 158.70(16)
C(1) Ir(1) C(2) 38.1(2)
C(1) Ir(1) C(3) 62.9(2)
C(1) Ir(1) C(4) 62.5(2)
C(1) Ir(1) C(5) 36.8(2)
C(2) Ir(1) C(3) 38.0(2)
C(2) Ir(1) C(4) 63.6(2)
C(2) Ir(1) C(5) 63.1(2)
C(3) Ir(1) C(4) 37.9(2)
C(3) Ir(1) C(5) 62.9(2)
C(4) Ir(1) C(5) 37.6(2)
Ir(1) W(1) S(1) 53.81(4)
Ir(1) W(1) S(2) 53.60(4)
Ir(1) W(1) O(1) 114.61(18)
Ir(1) W(1) O(2) 135.64(17)
S(1) W(1) S(2) 105.65(6)
S(1) W(1) O(1) 110.16(18)
S(1) W(1) O(2) 110.38(18)
S(2) W(1) O(1) 111.64(18)
S(2) W(1) O(2) 109.19(17)
O(1) W(1) O(2) 109.8(2)
Ir(1) S(1) W(1) 76.20(5)
Ir(1) S(2) W(1) 76.37(5)
Ir(1) P(1) C(11) 112.6(2)
Ir(1) P(1) C(12) 114.8(2)
Ir(1) P(1) C(13) 116.8(2)
C(11) P(1) C(12) 104.9(3)
C(11) P(1) C(13) 103.6(3)
C(12) P(1) C(13) 102.7(3)
Ir(1) C(1) C(2) 68.2(3)
Ir(1) C(1) C(5) 71.8(3)
Ir(1) C(1) C(6) 126.9(4)
C(2) C(1) C(5) 108.0(5)
C(2) C(1) C(6) 125.0(6)
C(5) C(1) C(6) 127.0(6)
Ir(1) C(2) C(1) 73.7(3)
Ir(1) C(2) C(3) 72.0(3)
Ir(1) C(2) C(7) 129.2(5)
C(1) C(2) C(3) 108.0(6)
C(1) C(2) C(7) 125.7(6)
C(3) C(2) C(7) 125.3(6)
Ir(1) C(3) C(2) 69.9(3)
Ir(1) C(3) C(4) 71.2(3)
Ir(1) C(3) C(8) 130.6(4)
C(2) C(3) C(4) 107.7(5)
C(2) C(3) C(8) 126.6(6)
C(4) C(3) C(8) 125.1(6)
Ir(1) C(4) C(3) 70.9(3)
Ir(1) C(4) C(5) 73.0(3)
Ir(1) C(4) C(9) 129.5(4)
C(3) C(4) C(5) 108.3(5)
C(3) C(4) C(9) 125.7(6)
C(5) C(4) C(9) 125.2(6)
Ir(1) C(5) C(1) 71.4(3)
Ir(1) C(5) C(4) 69.4(3)
Ir(1) C(5) C(10) 126.3(4)
C(1) C(5) C(4) 107.8(5)
C(1) C(5) C(10) 126.7(5)
C(4) C(5) C(10) 125.5(5)
C(1) C(6) H(1) 113.7
C(1) C(6) H(2) 108.6
C(1) C(6) H(3) 106.1
H(1) C(6) H(2) 109.5
H(1) C(6) H(3) 109.5
H(2) C(6) H(3) 109.5
C(2) C(7) H(4) 107.5
C(2) C(7) H(5) 107.9
C(2) C(7) H(6) 112.9
H(4) C(7) H(5) 109.5
H(4) C(7) H(6) 109.5
H(5) C(7) H(6) 109.5
C(3) C(8) H(7) 107.4
C(3) C(8) H(8) 113.0
C(3) C(8) H(9) 108.0
H(7) C(8) H(8) 109.5
H(7) C(8) H(9) 109.5
H(8) C(8) H(9) 109.5
C(4) C(9) H(10) 108.1
C(4) C(9) H(11) 109.2
C(4) C(9) H(12) 111.1
H(10) C(9) H(11) 109.5
H(10) C(9) H(12) 109.5
H(11) C(9) H(12) 109.5
C(5) C(10) H(13) 110.8
C(5) C(10) H(14) 109.1
C(5) C(10) H(15) 108.5
H(13) C(10) H(14) 109.5
H(13) C(10) H(15) 109.5
H(14) C(10) H(15) 109.5
P(1) C(11) H(16) 109.4
P(1) C(11) H(17) 109.8
P(1) C(11) H(18) 109.2
H(16) C(11) H(17) 109.5
H(16) C(11) H(18) 109.5
H(17) C(11) H(18) 109.5
P(1) C(12) H(19) 110.6
P(1) C(12) H(20) 108.5
P(1) C(12) H(21) 109.3
H(19) C(12) H(20) 109.5
H(19) C(12) H(21) 109.5
H(20) C(12) H(21) 109.5
P(1) C(13) H(22) 109.4
P(1) C(13) H(23) 110.9
P(1) C(13) H(24) 108.1
H(22) C(13) H(23) 109.5
H(22) C(13) H(24) 109.5
H(23) C(13) H(24) 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir(1) W(1) 2.8903(3)
Ir(1) S(1) 2.4019(17)
Ir(1) S(2) 2.3939(17)
Ir(1) P(1) 2.2901(19)
Ir(1) C(1) 2.264(6)
Ir(1) C(2) 2.190(6)
Ir(1) C(3) 2.217(6)
Ir(1) C(4) 2.221(6)
Ir(1) C(5) 2.269(6)
W(1) S(1) 2.2796(17)
W(1) S(2) 2.2795(18)
W(1) O(1) 1.737(5)
W(1) O(2) 1.743(4)
P(1) C(11) 1.823(7)
P(1) C(12) 1.813(7)
P(1) C(13) 1.817(7)
C(1) C(2) 1.456(9)
C(1) C(5) 1.430(9)
C(1) C(6) 1.495(9)
C(2) C(3) 1.435(9)
C(2) C(7) 1.488(10)
C(3) C(4) 1.441(9)
C(3) C(8) 1.475(9)
C(4) C(5) 1.449(9)
C(4) C(9) 1.478(9)
C(5) C(10) 1.491(9)
C(6) H(1) 0.950
C(6) H(2) 0.950
C(6) H(3) 0.950
C(7) H(4) 0.950
C(7) H(5) 0.950
C(7) H(6) 0.950
C(8) H(7) 0.950
C(8) H(8) 0.950
C(8) H(9) 0.950
C(9) H(10) 0.950
C(9) H(11) 0.950
C(9) H(12) 0.950
C(10) H(13) 0.950
C(10) H(14) 0.950
C(10) H(15) 0.950
C(11) H(16) 0.950
C(11) H(17) 0.950
C(11) H(18) 0.950
C(12) H(19) 0.950
C(12) H(20) 0.950
C(12) H(21) 0.950
C(13) H(22) 0.950
C(13) H(23) 0.950
C(13) H(24) 0.950
