#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/98/2009888.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009888
loop_
_publ_author_name
'Bachechi, Fiorella'
_publ_contact_author
;
     Dr. Fiorella Bachechi
     Istituto di Strutturistica Chimica
     "Giordano Giacomello", C.N.R
     Area della Ricerca di Roma
     P.O. Box 10
     I-00016 Monterotondo Stazione (Roma)
     Italy
;
_publ_section_title
;
 A tri-μ-chloro dirhodium (III) complex
 [Rh₂(μ-Cl)₃(triphos)₂](CF₃SO₃)₃ [triphos =
 CH₃C(CH₂PPh₂)₃]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1069
_journal_page_last               1072
_journal_paper_doi               10.1107/S0108270194001095
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C82 H78 Cl3 P6 Rh2,3C F3 O3 S'
_chemical_formula_sum            'C85 H78 Cl3 F9 O9 P6 Rh2 S3'
_chemical_formula_weight         2008.7
_chemical_name_systematic
;
tris(μ-chloro)-bis[1,1,1-tris(diphenylphosphinomethyl)ethane-
P, P', P'']dirhodium(III) trifluoromethanesulfonate
;
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3 '
_symmetry_space_group_name_H-M   'P a -3'
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            8.00
_cell_length_a                   26.430(6)
_cell_length_b                   26.430(6)
_cell_length_c                   26.430(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      14.0
_cell_volume                     18463(7)
_computing_structure_refinement  'CAOS (Cerrini & Spagna, 1977)'
_computing_structure_solution    'CAOS (Cerrini & Spagna, 1977)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Syntex P2₁'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6681
_diffrn_reflns_theta_max         28.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        8.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.6776
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   'empirical with \y-scan at \c=90\%, normal'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       Prism
_exptl_crystal_F_000             8160
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.28
_refine_ls_goodness_of_fit_obs   4.12
_refine_ls_hydrogen_treatment    'riding on the parent carbon atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         1792
_refine_ls_R_factor_obs          0.0680
_refine_ls_shift/esd_max         0.90
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'sigma w = 1/\s^2^(F^2^)'
_refine_ls_wR_factor_obs         0.0759
_reflns_number_observed          1782
_reflns_number_total             3893
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            na1075.cif
_cod_data_source_block           BACHECHI
_cod_original_cell_volume        18462(7)
_cod_original_sg_symbol_H-M      'P a  -3 '
_cod_database_code               2009888
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Rh(1) 0.22190(10) 0.22190(10) 0.22190(10) 0.0340(10) ?
Rh(2) 0.29650(10) 0.29650(10) 0.29650(10) 0.0350(10) ?
C(14) 0.1435(8) 0.1435(8) 0.1435(8) 0.050(10) ?
C(15) 0.1101(8) 0.1101(8) 0.1101(8) 0.060(10) ?
C(24) 0.3773(8) 0.3773(8) 0.3773(8) 0.050(10) ?
C(25) 0.4094(8) 0.4094(8) 0.4094(8) 0.060(10) ?
P(1) 0.2110(2) 0.1352(2) 0.2314(2) 0.041(2) ?
P(4) 0.3824(2) 0.3105(2) 0.2856(2) 0.045(2) ?
Cl(1) 0.2123(2) 0.2568(2) 0.3080(2) 0.045(2) ?
C(11) 0.1627(7) 0.1083(7) 0.1870(7) 0.050(10) ?
C(16) 0.1917(6) 0.1117(6) 0.2946(7) 0.040(10) ?
C(17) 0.2139(8) 0.1312(8) 0.3388(8) 0.070(10) ?
C(18) 0.2030(10) 0.1155(9) 0.3860(8) 0.070(10) ?
C(19) 0.1690(10) 0.0745(9) 0.3910(10) 0.070(10) ?
C(110) 0.1490(10) 0.0538(9) 0.3500(10) 0.080(10) ?
C(111) 0.1609(7) 0.0705(7) 0.3006(8) 0.060(10) ?
C(112) 0.2700(7) 0.0991(7) 0.2182(9) 0.060(10) ?
C(113) 0.3051(7) 0.0911(8) 0.2581(8) 0.060(10) ?
C(114) 0.3504(9) 0.0676(9) 0.2470(10) 0.070(10) ?
C(115) 0.3612(8) 0.0516(9) 0.2000(10) 0.070(10) ?
C(116) 0.3287(7) 0.0581(8) 0.1620(10) 0.070(10) ?
C(117) 0.2818(7) 0.0817(7) 0.1704(9) 0.070(10) ?
C(21) 0.4074(8) 0.3578(7) 0.3323(8) 0.050(10) ?
C(26) 0.4190(7) 0.2518(7) 0.2933(9) 0.050(10) ?
C(27) 0.4414(7) 0.2408(8) 0.3391(9) 0.060(10) ?
C(28) 0.4680(8) 0.1942(9) 0.3442(9) 0.070(10) ?
C(29) 0.4728(8) 0.1622(9) 0.3050(10) 0.080(10) ?
C(210) 0.4532(7) 0.1734(8) 0.2609(9) 0.070(10) ?
C(211) 0.4260(8) 0.2197(8) 0.2535(9) 0.070(10) ?
C(212) 0.4077(9) 0.3320(7) 0.2262(9) 0.060(10) ?
C(213) 0.4600(8) 0.3399(8) 0.2180(10) 0.070(10) ?
C(214) 0.4780(10) 0.3570(10) 0.1700(10) 0.09(2) ?
C(215) 0.4540(10) 0.3630(10) 0.131(2) 0.080(10) ?
C(216) 0.408(2) 0.3590(10) 0.1350(10) 0.08(2) ?
C(217) 0.3796(9) 0.3409(9) 0.1830(10) 0.080(10) ?
S(1) 0.0249(3) 0.0232(3) 0.2588(3) 0.085(3) ?
C(42) -0.0120(10) 0.0000(10) 0.2100(10) 0.090(10) ?
O(1) 0.0562(6) 0.0573(6) 0.2306(7) 0.090(10) ?
O(2) -0.0104(7) 0.0453(8) 0.2935(9) 0.130(10) ?
O(3) 0.0489(7) -0.0207(7) 0.2808(8) 0.110(10) ?
F(1) -0.0408(6) 0.0336(7) 0.1861(7) 0.120(10) ?
F(2) 0.0111(8) -0.0252(7) 0.1737(7) 0.140(10) ?
F(3) -0.0458(8) -0.0360(8) 0.2272(8) 0.160(10) ?
H(1) 0.2363(8) 0.1589(8) 0.3334(8) ? ?
H(2) 0.2200(10) 0.1315(9) 0.4145(8) ? ?
H(3) 0.1610(10) 0.0610(9) 0.4240(10) ? ?
H(4) 0.1250(10) 0.0270(9) 0.3540(10) ? ?
H(5) 0.1463(7) 0.0551(7) 0.2715(8) ? ?
H(6) 0.2985(7) 0.1021(8) 0.2917(8) ? ?
H(7) 0.3745(9) 0.0615(9) 0.2730(10) ? ?
H(8) 0.3930(8) 0.0365(9) 0.1920(10) ? ?
H(9) 0.3368(7) 0.0461(8) 0.1290(10) ? ?
H(10) 0.2577(7) 0.0860(7) 0.1438(9) ? ?
H(11) 0.4399(7) 0.2636(8) 0.3678(9) ? ?
H(12) 0.4842(8) 0.1859(9) 0.3754(9) ? ?
H(13) 0.4892(8) 0.1301(9) 0.3090(10) ? ?
H(14) 0.4583(7) 0.1508(8) 0.2330(9) ? ?
H(15) 0.4131(8) 0.2274(8) 0.2204(9) ? ?
H(16) 0.4816(8) 0.3320(8) 0.2460(10) ? ?
H(17) 0.5130(10) 0.3670(10) 0.1700(10) ? ?
H(18) 0.4700(10) 0.3670(10) 0.099(2) ? ?
H(19) 0.388(2) 0.3700(10) 0.1060(10) ? ?
H(20) 0.3439(9) 0.3368(9) 0.1840(10) ? ?
H(21) 0.0980 0.1300 0.0820 ? ?
H(24) 0.3910 0.4230 0.4380 ? ?
H(27) 0.1336(7) 0.1007(7) 0.2068(7) ? ?
H(28) 0.1756(7) 0.0777(7) 0.1728(7) ? ?
H(29) 0.4182(8) 0.3866(7) 0.3134(8) ? ?
H(30) 0.4362(8) 0.3416(7) 0.3464(8) ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C Carbon .002 .002 'IntTabIV  Tab.2.2A 2.3.1'
O Oxygen .008 .006 'IntTabIV  Tab.2.2A 2.3.1'
H Hydrogen .000 .000 'IntTabIV  Tab.2.2C      '
F Fluorine .014 .010 'IntTabIV  Tab.2.2A 2.3.1'
P Phosphorus .090 .095 'IntTabIV  Tab.2.2A 2.3.1'
S Sulfur .110 .124 'IntTabIV  Tab.2.2A 2.3.1'
Cl Chlorine .132 .159 'IntTabIV  Tab.2.2A 2.3.1'
Rh Rhodium -1.287 .919 'IntTabIV  Tab.2.2A 2.3.1'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 0 1
0 2 2
1 2 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Rh(1) Cl(1) Rh(2) 87.30(10) yes
Cl(1) Rh(1) Cl(1') 77.80(10) yes
Cl(1) Rh(2) Cl(1') 77.40(10) yes
P(1) Rh(1) P(1') 89.90(10) yes
P(1) Rh(1) Cl(1) 104.8(2) yes
P(1) Rh(1) Cl(1') 88.40(10) yes
P(1) Rh(1) Cl(1") 165.20(10) yes
P(4) Rh(2) P(4') 89.10(10) yes
P(4) Rh(2) Cl(1) 164.2(2) yes
P(4) Rh(2) Cl(1') 88.30(10) yes
P(4) Rh(2) Cl(1") 106.50(10) yes
C(16) P(1) C(11) 104.5(8) yes
C(112) P(1) C(11) 104.8(9) yes
C(112) P(1) C(16) 103.1(9) yes
C(26) P(4) C(21) 107.7(9) yes
C(212) P(4) C(21) 103.4(9) yes
C(212) P(4) C(26) 99.5(9) yes
C(11) C(14) C(15) 105.0(10) yes
P(1) C(11) C(14) 117.0(10) yes
C(17) C(16) P(1) 120.0(10) yes
C(111) C(16) P(1) 122.0(10) yes
C(113) C(112) P(1) 118.0(10) yes
C(117) C(112) P(1) 122.0(10) yes
C(21) C(24) C(25) 110.0(10) yes
P(4) C(21) C(24) 123.0(10) yes
C(27) C(26) P(4) 119.0(10) yes
C(211) C(26) P(4) 120.0(10) yes
C(213) C(212) P(4) 123.0(10) yes
C(217) C(212) P(4) 125.0(10) yes
C(111) C(16) C(17) 116.0(10) no
C(18) C(17) C(16) 124(2) no
C(19) C(18) C(17) 117(2) no
C(110) C(19) C(18) 118(2) no
C(111) C(110) C(19) 123(2) no
C(110) C(111) C(16) 119.0(10) no
C(117) C(112) C(113) 118.0(10) no
C(114) C(113) C(112) 118(2) no
C(115) C(114) C(113) 121(2) no
C(116) C(115) C(114) 121(2) no
C(117) C(116) C(115) 121(2) no
C(116) C(117) C(112) 119(2) no
C(211) C(26) C(27) 119.0(10) no
C(28) C(27) C(26) 118(2) no
C(29) C(28) C(27) 121(2) no
C(210) C(29) C(28) 120(2) no
C(211) C(210) C(29) 120(2) no
C(210) C(211) C(26) 119(2) no
C(217) C(212) C(213) 111(2) no
C(214) C(213) C(212) 120(2) no
C(215) C(214) C(213) 128(3) no
C(216) C(215) C(214) 114(3) no
C(217) C(216) C(215) 125(3) no
C(216) C(217) C(212) 118(2) no
O(1) S(1) C(42) 99.0(10) no
O(2) S(1) C(42) 104.0(10) no
O(2) S(1) O(1) 116.0(10) no
O(3) S(1) C(42) 104.0(10) no
O(3) S(1) O(1) 117.0(10) no
O(3) S(1) O(2) 110.0(10) no
F(1) C(42) S(1) 115(2) no
F(2) C(42) S(1) 117(2) no
F(2) C(42) F(1) 104(2) no
F(3) C(42) S(1) 112(2) no
F(3) C(42) F(1) 104(2) no
F(3) C(42) F(2) 101(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Rh(1) Rh(2) 3.4140(10) yes
Rh(1) P(1) 2.321(5) yes
Rh(1) Cl(1) 2.469(5) yes
Rh(2) P(4) 2.319(4) yes
Rh(2) Cl(1) 2.478(5) yes
P(1) C(11) 1.870(10) yes
P(1) C(16) 1.850(10) yes
P(1) C(112) 1.86(2) yes
P(4) C(21) 1.87(2) yes
P(4) C(26) 1.840(10) yes
P(4) C(212) 1.79(2) yes
C(14) C(15) 1.52(2) yes
C(14) C(11) 1.56(2) yes
C(24) C(25) 1.46(2) yes
C(24) C(21) 1.52(2) yes
C(16) C(17) 1.40(2) no
C(16) C(111) 1.36(2) no
C(17) C(18) 1.34(2) no
C(18) C(19) 1.42(3) no
C(19) C(110) 1.33(3) no
C(110) C(111) 1.39(3) no
C(112) C(113) 1.41(3) no
C(112) C(117) 1.37(3) no
C(113) C(114) 1.37(3) no
C(114) C(115) 1.35(3) no
C(115) C(116) 1.32(3) no
C(116) C(117) 1.40(2) no
C(26) C(27) 1.37(3) no
C(26) C(211) 1.36(3) no
C(27) C(28) 1.42(3) no
C(28) C(29) 1.34(3) no
C(29) C(210) 1.31(3) no
C(210) C(211) 1.43(2) no
C(212) C(213) 1.41(3) no
C(212) C(217) 1.38(3) no
C(213) C(214) 1.42(4) no
C(214) C(215) 1.21(5) no
C(215) C(216) 1.25(5) no
C(216) C(217) 1.54(4) no
S(1) C(42) 1.72(3) no
S(1) O(1) 1.430(10) no
S(1) O(2) 1.43(2) no
S(1) O(3) 1.44(2) no
C(42) F(1) 1.34(3) no
C(42) F(2) 1.32(3) no
C(42) F(3) 1.37(3) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
P(1) Rh(1) Rh(2) P(4) 86.0(2)
P(1) Rh(1) Rh(2) P(4') -156.0(2)
P(1) Rh(1) Rh(2) P(4) -34.0(2)
