#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/4/4060553.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_4060553
_journal_name_full  'Organometallics'
_journal_year       2005
_publ_section_title
;
 Iminophosphorane-based nucleophilic ruthenium(II) carbene complexes:
 An unusual C-C coupling and C-H activation by the addition of alkynes
 to the Ru=C bond
;
loop_
_publ_author_name
  'Victorio Cadierno'
  'Josefina D\'iez'
  'Joaqu\'in Garc\'ia-\'Alvarez'
  'Jos\'e Gimeno'
_chemical_formula_sum 'C54 H46 N5 O Rh'
_chemical_formula_weight  883.87
_symmetry_cell_setting  TRICLINIC
_symmetry_space_group_name_H-M  'P -1'
loop_
_symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a  13.263(3)
_cell_length_b  13.699(3)
_cell_length_c  14.462(3)
_cell_angle_alpha  94.28(3)
_cell_angle_beta  100.58(3)
_cell_angle_gamma  113.76(3)
_cell_volume  2331.5(8)
_cell_formula_units_Z  2
_cell_measurement_temperature  293(2)
_exptl_crystal_density_diffrn  1.259
_diffrn_ambient_temperature  293(2)
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
Rh1 Rh 0.47968(3) 0.80035(3) 0.50051(2) 0.04767(18) Uani 1 1 d . . .
O1 O 0.3388(5) 0.5720(5) 0.7797(4) 0.1023(15) Uani 1 1 d . . .
N1 N 0.5957(3) 0.8528(3) 0.6263(3) 0.0519(9) Uani 1 1 d . . .
N2 N 0.4129(3) 0.8997(3) 0.5428(3) 0.0518(9) Uani 1 1 d . . .
N3 N 0.3597(3) 0.7468(3) 0.3767(3) 0.0513(8) Uani 1 1 d . . .
N4 N 0.5553(3) 0.7120(3) 0.4520(3) 0.0527(9) Uani 1 1 d . . .
N5 N 0.2383(4) 0.5862(4) 0.6396(3) 0.0691(11) Uani 1 1 d . . .
C1 C 0.6800(4) 0.8183(4) 0.6540(3) 0.0553(11) Uani 1 1 d . . .
C2 C 0.7292(4) 0.8561(4) 0.7543(3) 0.0601(11) Uani 1 1 d . . .
H2A H 0.7867 0.8432 0.7906 0.072 Uiso 1 1 calc R . .
C3 C 0.6766(4) 0.9141(4) 0.7866(3) 0.0577(11) Uani 1 1 d . . .
H3A H 0.6906 0.9472 0.8490 0.069 Uiso 1 1 calc R . .
C4 C 0.5956(4) 0.9143(4) 0.7065(3) 0.0529(10) Uani 1 1 d . . .
C5 C 0.5312(4) 0.9746(4) 0.7066(3) 0.0518(10) Uani 1 1 d . . .
C6 C 0.5399(4) 1.0396(4) 0.7988(3) 0.0532(10) Uani 1 1 d . . .
C7 C 0.6400(4) 1.1185(4) 0.8535(3) 0.0609(12) Uani 1 1 d . . .
H7A H 0.7061 1.1353 0.8321 0.073 Uiso 1 1 calc R . .
C8 C 0.6448(5) 1.1734(5) 0.9397(4) 0.0674(13) Uani 1 1 d . . .
H8A H 0.7140 1.2260 0.9753 0.081 Uiso 1 1 calc R . .
C9 C 0.5487(5) 1.1513(5) 0.9734(4) 0.0669(13) Uani 1 1 d . . .
C10 C 0.4478(5) 1.0737(6) 0.9179(4) 0.0754(15) Uani 1 1 d . . .
H10A H 0.3816 1.0585 0.9388 0.090 Uiso 1 1 calc R . .
C11 C 0.4420(5) 1.0177(5) 0.8319(4) 0.0644(12) Uani 1 1 d . . .
H11A H 0.3727 0.9653 0.7962 0.077 Uiso 1 1 calc R . .
C12 C 0.5552(8) 1.2142(7) 1.0683(5) 0.095(2) Uani 1 1 d . . .
H12A H 0.6324 1.2644 1.0960 0.143 Uiso 1 1 calc R . .
H12B H 0.5284 1.1646 1.1111 0.143 Uiso 1 1 calc R . .
H12C H 0.5090 1.2529 1.0572 0.143 Uiso 1 1 calc R . .
C13 C 0.4545(4) 0.9749(4) 0.6265(3) 0.0522(10) Uani 1 1 d . . .
C14 C 0.3987(4) 1.0451(4) 0.6204(3) 0.0552(10) Uani 1 1 d . . .
H14A H 0.4144 1.1046 0.6653 0.066 Uiso 1 1 calc R . .
C15 C 0.3190(4) 1.0090(4) 0.5374(3) 0.0553(10) Uani 1 1 d . . .
H15A H 0.2697 1.0393 0.5153 0.066 Uiso 1 1 calc R . .
C16 C 0.3237(4) 0.9157(4) 0.4892(3) 0.0517(10) Uani 1 1 d . . .
C17 C 0.2472(4) 0.8463(4) 0.4083(3) 0.0520(10) Uani 1 1 d . . .
C18 C 0.1376(4) 0.8570(4) 0.3781(3) 0.0534(10) Uani 1 1 d . . .
C19 C 0.0712(4) 0.8517(4) 0.4425(4) 0.0606(11) Uani 1 1 d . . .
H19A H 0.0967 0.8447 0.5049 0.073 Uiso 1 1 calc R . .
C20 C -0.0333(4) 0.8565(5) 0.4165(4) 0.0639(12) Uani 1 1 d . . .
H20A H -0.0754 0.8542 0.4618 0.077 Uiso 1 1 calc R . .
C21 C -0.0743(4) 0.8647(5) 0.3236(4) 0.0642(12) Uani 1 1 d . . .
C22 C -0.0070(4) 0.8716(5) 0.2593(4) 0.0634(12) Uani 1 1 d . . .
H22A H -0.0327 0.8781 0.1967 0.076 Uiso 1 1 calc R . .
C23 C 0.0982(4) 0.8688(4) 0.2860(4) 0.0606(11) Uani 1 1 d . . .
H23A H 0.1422 0.8750 0.2416 0.073 Uiso 1 1 calc R . .
C24 C -0.1884(5) 0.8663(6) 0.2928(6) 0.0859(19) Uani 1 1 d . . .
H24A H -0.2025 0.8721 0.2264 0.129 Uiso 1 1 calc R . .
H24B H -0.1894 0.9272 0.3296 0.129 Uiso 1 1 calc R . .
H24C H -0.2462 0.8008 0.3030 0.129 Uiso 1 1 calc R . .
C25 C 0.2629(4) 0.7642(4) 0.3573(3) 0.0518(10) Uani 1 1 d . . .
C26 C 0.1842(4) 0.6889(4) 0.2749(4) 0.0593(11) Uani 1 1 d . . .
H26A H 0.1115 0.6817 0.2491 0.071 Uiso 1 1 calc R . .
C27 C 0.2350(4) 0.6307(4) 0.2419(4) 0.0602(11) Uani 1 1 d . . .
H27A H 0.2043 0.5772 0.1882 0.072 Uiso 1 1 calc R . .
C28 C 0.3453(4) 0.6660(4) 0.3046(3) 0.0546(10) Uani 1 1 d . . .
C29 C 0.4239(4) 0.6249(4) 0.2951(3) 0.0549(11) Uani 1 1 d . . .
C30 C 0.3991(4) 0.5486(4) 0.2041(4) 0.0570(11) Uani 1 1 d . . .
C31 C 0.3887(5) 0.5840(5) 0.1172(4) 0.0681(13) Uani 1 1 d . . .
H31A H 0.3970 0.6545 0.1154 0.082 Uiso 1 1 calc R . .
C32 C 0.3662(5) 0.5161(5) 0.0333(4) 0.0737(15) Uani 1 1 d . . .
H32A H 0.3591 0.5419 -0.0242 0.088 Uiso 1 1 calc R . .
C33 C 0.3541(5) 0.4129(5) 0.0323(4) 0.0713(15) Uani 1 1 d . . .
C34 C 0.3661(5) 0.3757(5) 0.1190(4) 0.0692(13) Uani 1 1 d . . .
H34A H 0.3580 0.3052 0.1201 0.083 Uiso 1 1 calc R . .
C35 C 0.3905(5) 0.4448(5) 0.2042(4) 0.0635(12) Uani 1 1 d . . .
H35A H 0.4011 0.4205 0.2619 0.076 Uiso 1 1 calc R . .
C36 C 0.3292(6) 0.3381(6) -0.0614(5) 0.094(2) Uani 1 1 d . . .
H36A H 0.3251 0.3765 -0.1139 0.141 Uiso 1 1 calc R . .
H36B H 0.2584 0.2762 -0.0690 0.141 Uiso 1 1 calc R . .
H36C H 0.3887 0.3149 -0.0601 0.141 Uiso 1 1 calc R . .
C37 C 0.5233(4) 0.6485(4) 0.3643(3) 0.0545(10) Uani 1 1 d . . .
C38 C 0.6065(4) 0.6085(5) 0.3553(4) 0.0627(12) Uani 1 1 d . . .
H38A H 0.6061 0.5657 0.3021 0.075 Uiso 1 1 calc R . .
C39 C 0.6848(4) 0.6444(5) 0.4379(4) 0.0628(12) Uani 1 1 d . . .
H39A H 0.7484 0.6304 0.4521 0.075 Uiso 1 1 calc R . .
C40 C 0.6545(4) 0.7081(4) 0.5006(4) 0.0566(11) Uani 1 1 d . . .
C41 C 0.7106(4) 0.7563(4) 0.5948(4) 0.0555(11) Uani 1 1 d . . .
C42 C 0.8172(4) 0.7436(4) 0.6359(3) 0.0558(11) Uani 1 1 d . . .
C43 C 0.8186(5) 0.6468(5) 0.6502(4) 0.0667(13) Uani 1 1 d . . .
H43A H 0.7519 0.5836 0.6323 0.080 Uiso 1 1 calc R . .
C44 C 0.9207(5) 0.6427(5) 0.6920(4) 0.0743(15) Uani 1 1 d . . .
H44A H 0.9201 0.5760 0.7012 0.089 Uiso 1 1 calc R . .
C45 C 1.0196(5) 0.7317(6) 0.7193(4) 0.0725(15) Uani 1 1 d . . .
C46 C 1.0187(5) 0.8305(5) 0.7023(4) 0.0763(15) Uani 1 1 d . . .
H46A H 1.0863 0.8928 0.7188 0.092 Uiso 1 1 calc R . .
C47 C 0.9211(4) 0.8377(5) 0.6621(4) 0.0675(13) Uani 1 1 d . . .
H47A H 0.9227 0.9045 0.6518 0.081 Uiso 1 1 calc R . .
C48 C 1.1300(6) 0.7287(8) 0.7688(6) 0.106(3) Uani 1 1 d . . .
H48A H 1.1165 0.6556 0.7756 0.160 Uiso 1 1 calc R . .
H48B H 1.1580 0.7730 0.8306 0.160 Uiso 1 1 calc R . .
H48C H 1.1850 0.7556 0.7312 0.160 Uiso 1 1 calc R . .
C49 C 0.3828(5) 0.6666(4) 0.5505(4) 0.0635(12) Uani 1 1 d . . .
H49A H 0.3277 0.6139 0.4969 0.076 Uiso 1 1 calc R . .
H49B H 0.4313 0.6348 0.5803 0.076 Uiso 1 1 calc R . .
C50 C 0.3208(5) 0.6881(5) 0.6215(5) 0.0739(15) Uani 1 1 d . . .
H50A H 0.3748 0.7291 0.6808 0.089 Uiso 1 1 calc R . .
H50B H 0.2821 0.7309 0.5969 0.089 Uiso 1 1 calc R . .
C51 C 0.1280(6) 0.5321(6) 0.5768(6) 0.091(2) Uani 1 1 d . . .
H51A H 0.1333 0.5085 0.5137 0.110 Uiso 1 1 calc R . .
H51B H 0.0900 0.5796 0.5717 0.110 Uiso 1 1 calc R . .
C52 C 0.0649(7) 0.4360(7) 0.6217(8) 0.114(3) Uani 1 1 d . . .
H52A H -0.0024 0.4396 0.6358 0.137 Uiso 1 1 calc R . .
H52B H 0.0423 0.3690 0.5790 0.137 Uiso 1 1 calc R . .
C53 C 0.1433(7) 0.4419(6) 0.7092(6) 0.096(2) Uani 1 1 d . . .
H53A H 0.1562 0.3770 0.7075 0.115 Uiso 1 1 calc R . .
H53B H 0.1126 0.4488 0.7640 0.115 Uiso 1 1 calc R . .
C54 C 0.2529(6) 0.5401(5) 0.7158(5) 0.0739(15) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0520(2) 0.0460(3) 0.0506(2) 0.00588(16) 0.01920(16) 0.02367(17)
O1 0.129(4) 0.101(4) 0.086(3) 0.010(3) 0.029(3) 0.058(3)
N1 0.059(2) 0.048(2) 0.059(2) 0.0098(16) 0.0219(17) 0.0294(17)
N2 0.0538(19) 0.053(2) 0.0527(19) 0.0084(16) 0.0163(16) 0.0257(16)
N3 0.0540(19) 0.046(2) 0.059(2) 0.0051(16) 0.0216(16) 0.0231(16)
N4 0.057(2) 0.052(2) 0.054(2) 0.0064(16) 0.0183(16) 0.0260(17)
N5 0.068(3) 0.061(3) 0.080(3) 0.014(2) 0.034(2) 0.022(2)
C1 0.061(3) 0.056(3) 0.056(2) 0.012(2) 0.0179(19) 0.030(2)
C2 0.069(3) 0.063(3) 0.055(2) 0.011(2) 0.017(2) 0.034(2)
C3 0.067(3) 0.061(3) 0.054(2) 0.011(2) 0.021(2) 0.032(2)
C4 0.057(2) 0.057(3) 0.049(2) 0.0089(18) 0.0195(18) 0.027(2)
C5 0.058(2) 0.053(3) 0.048(2) 0.0036(18) 0.0189(18) 0.0246(19)
C6 0.063(2) 0.053(3) 0.053(2) 0.0090(19) 0.0231(19) 0.030(2)
C7 0.066(3) 0.063(3) 0.060(3) 0.007(2) 0.025(2) 0.030(2)
C8 0.081(3) 0.062(4) 0.058(3) 0.001(2) 0.010(2) 0.034(3)
C9 0.099(4) 0.060(3) 0.057(3) 0.012(2) 0.030(3) 0.044(3)
C10 0.084(4) 0.089(4) 0.070(3) 0.015(3) 0.041(3) 0.043(3)
C11 0.069(3) 0.065(3) 0.065(3) 0.008(2) 0.028(2) 0.030(2)
C12 0.144(6) 0.099(6) 0.065(3) 0.011(3) 0.042(4) 0.068(5)
C13 0.054(2) 0.051(3) 0.056(2) 0.0055(18) 0.0199(18) 0.0249(19)
C14 0.061(2) 0.049(3) 0.060(2) 0.0008(19) 0.019(2) 0.027(2)
C15 0.061(2) 0.054(3) 0.060(2) 0.0077(19) 0.019(2) 0.032(2)
C16 0.055(2) 0.056(3) 0.056(2) 0.0114(19) 0.0228(18) 0.030(2)
C17 0.050(2) 0.055(3) 0.056(2) 0.0113(19) 0.0192(18) 0.0255(19)
C18 0.053(2) 0.051(3) 0.059(2) 0.0066(19) 0.0171(19) 0.0242(19)
C19 0.058(2) 0.067(3) 0.061(3) 0.007(2) 0.021(2) 0.029(2)
C20 0.061(3) 0.069(4) 0.069(3) 0.009(2) 0.027(2) 0.030(2)
C21 0.055(3) 0.056(3) 0.082(3) 0.004(2) 0.018(2) 0.025(2)
C22 0.067(3) 0.068(4) 0.063(3) 0.012(2) 0.017(2) 0.034(2)
C23 0.059(3) 0.067(3) 0.061(3) 0.010(2) 0.023(2) 0.029(2)
C24 0.064(3) 0.088(5) 0.115(5) 0.013(4) 0.023(3) 0.041(3)
C25 0.050(2) 0.054(3) 0.053(2) 0.0062(18) 0.0194(18) 0.0204(19)
C26 0.053(2) 0.060(3) 0.064(3) 0.003(2) 0.018(2) 0.022(2)
C27 0.061(3) 0.057(3) 0.062(3) -0.002(2) 0.017(2) 0.025(2)
C28 0.059(2) 0.049(3) 0.055(2) 0.0022(18) 0.0191(19) 0.0206(19)
C29 0.063(3) 0.051(3) 0.057(2) 0.0042(19) 0.024(2) 0.026(2)
C30 0.063(3) 0.049(3) 0.061(3) 0.000(2) 0.020(2) 0.025(2)
C31 0.082(3) 0.065(4) 0.063(3) 0.009(2) 0.025(2) 0.034(3)
C32 0.092(4) 0.075(4) 0.059(3) 0.009(2) 0.024(3) 0.038(3)
C33 0.073(3) 0.080(4) 0.058(3) -0.009(2) 0.019(2) 0.032(3)
C34 0.079(3) 0.053(3) 0.082(3) 0.001(2) 0.029(3) 0.032(2)
C35 0.075(3) 0.060(3) 0.061(3) 0.006(2) 0.021(2) 0.032(2)
C36 0.102(5) 0.098(5) 0.073(4) -0.023(3) 0.018(3) 0.040(4)
C37 0.062(3) 0.050(3) 0.058(2) 0.0046(19) 0.023(2) 0.028(2)
C38 0.067(3) 0.061(3) 0.069(3) 0.001(2) 0.024(2) 0.035(2)
C39 0.061(3) 0.065(3) 0.073(3) 0.003(2) 0.022(2) 0.036(2)
C40 0.056(2) 0.055(3) 0.067(3) 0.010(2) 0.022(2) 0.029(2)
C41 0.057(2) 0.057(3) 0.063(3) 0.013(2) 0.020(2) 0.032(2)
C42 0.060(2) 0.057(3) 0.060(3) 0.009(2) 0.019(2) 0.032(2)
C43 0.066(3) 0.062(4) 0.082(3) 0.015(3) 0.025(2) 0.034(2)
C44 0.080(3) 0.075(4) 0.086(4) 0.014(3) 0.022(3) 0.050(3)
C45 0.070(3) 0.089(5) 0.074(3) 0.009(3) 0.019(3) 0.049(3)
C46 0.059(3) 0.079(4) 0.086(4) 0.004(3) 0.018(3) 0.026(3)
C47 0.067(3) 0.062(3) 0.077(3) 0.012(2) 0.021(2) 0.029(2)
C48 0.081(4) 0.136(8) 0.117(6) 0.003(5) 0.010(4) 0.069(5)
C49 0.073(3) 0.055(3) 0.068(3) 0.011(2) 0.030(2) 0.026(2)
C50 0.079(3) 0.060(4) 0.086(4) 0.011(3) 0.044(3) 0.022(3)
C51 0.077(4) 0.081(5) 0.103(5) 0.019(4) 0.030(3) 0.017(3)
C52 0.084(4) 0.084(6) 0.174(9) 0.037(5) 0.052(5) 0.021(4)
C53 0.120(6) 0.072(5) 0.113(5) 0.034(4) 0.065(5) 0.038(4)
C54 0.090(4) 0.066(4) 0.077(4) 0.008(3) 0.037(3) 0.038(3)
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
Rh1 N2 2.014(4) . ?
Rh1 N4 2.019(4) . ?
Rh1 N1 2.020(4) . ?
Rh1 N3 2.023(4) . ?
Rh1 C49 2.043(5) . ?
O1 C54 1.223(8) . ?
N1 C4 1.383(6) . ?
N1 C1 1.387(6) . ?
N2 C13 1.393(6) . ?
N2 C16 1.395(6) . ?
N3 C25 1.382(6) . ?
N3 C28 1.391(6) . ?
N4 C37 1.373(6) . ?
N4 C40 1.396(6) . ?
N5 C54 1.332(8) . ?
N5 C51 1.432(8) . ?
N5 C50 1.465(7) . ?
C1 C41 1.383(7) . ?
C1 C2 1.438(7) . ?
C2 C3 1.358(7) . ?
C3 C4 1.429(7) . ?
C4 C5 1.407(7) . ?
C5 C13 1.396(7) . ?
C5 C6 1.508(6) . ?
C6 C7 1.373(7) . ?
C6 C11 1.392(7) . ?
C7 C8 1.384(7) . ?
C8 C9 1.376(8) . ?
C9 C10 1.378(9) . ?
C9 C12 1.533(8) . ?
C10 C11 1.385(7) . ?
C13 C14 1.428(7) . ?
C14 C15 1.352(7) . ?
C15 C16 1.439(7) . ?
C16 C17 1.386(7) . ?
C17 C25 1.405(7) . ?
C17 C18 1.507(6) . ?
C18 C19 1.383(7) . ?
C18 C23 1.385(7) . ?
C19 C20 1.397(7) . ?
C20 C21 1.385(8) . ?
C21 C22 1.386(7) . ?
C21 C24 1.507(7) . ?
C22 C23 1.395(7) . ?
C25 C26 1.437(7) . ?
C26 C27 1.345(7) . ?
C27 C28 1.440(7) . ?
C28 C29 1.391(7) . ?
C29 C37 1.403(7) . ?
C29 C30 1.513(6) . ?
C30 C35 1.379(8) . ?
C30 C31 1.384(8) . ?
C31 C32 1.379(8) . ?
C32 C33 1.356(9) . ?
C33 C34 1.394(9) . ?
C33 C36 1.534(7) . ?
C34 C35 1.397(7) . ?
C37 C38 1.437(7) . ?
C38 C39 1.338(7) . ?
C39 C40 1.430(7) . ?
C40 C41 1.394(7) . ?
C41 C42 1.513(6) . ?
C42 C43 1.364(8) . ?
C42 C47 1.417(8) . ?
C43 C44 1.403(8) . ?
C44 C45 1.346(9) . ?
C45 C46 1.397(9) . ?
C45 C48 1.526(8) . ?
C46 C47 1.363(8) . ?
C49 C50 1.509(7) . ?
C51 C52 1.515(10) . ?
C52 C53 1.458(12) . ?
C53 C54 1.512(10) . ?