#------------------------------------------------------------------------------
#$Date: 2010-12-09 18:44:53 +0000 (Thu, 09 Dec 2010) $
#$Revision: 3898 $
#$URL: svn://www.crystallography.net/cod/cif/7/7051241.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_7051241
loop_
_publ_author_name
'Joseph N. Coalter III'
'John C. Bollinger'
'John C. Huffman'
'Ulrike Werner--Zwanziger'
'Kenneth G. Caulton'
'Ernest R. Davidson'
'H\'el\`ene G\'erard'
'Eric Clot'
'Odile Eisenstein'
_publ_section_title
;
 Coordinated carbenes from electron-rich olefins on RuHCl(PPr3i)2
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              9
_journal_page_last               26
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C18 H43 Cl N2 P2 Ru'
_chemical_formula_weight         486.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9985(10)
_cell_length_b                   8.9047(11)
_cell_length_c                   16.614(2)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    100
_cell_measurement_theta_max      12.36
_cell_measurement_theta_min      9.66
_cell_volume                     1182.5(3)
_computing_cell_refinement       'XTEL library'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL library'
_computing_molecular_graphics    'XTEL library'
_computing_publication_material  'XTEL library'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measurement_device       'Picker diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3678
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.918
_refine_ls_goodness_of_fit_obs   0.955
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_restrained_S_obs      0.955
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_obs          0.0346
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc
   w = [\s^2^(Fo^2^)+(0.0400Fo^2^)^2^]^-1^
;
_refine_ls_wR_factor_all         0.0778
_refine_ls_wR_factor_obs         0.0675
_reflns_number_observed          1487
_reflns_number_total             2049
_reflns_observed_criterion       2sigma(I)
_[local]_cod_data_source_file    a907624g.txt
_[local]_cod_data_source_block   98022
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_cod_original_cell_volume        1182.5(2)
_cod_database_code               7051241
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ru1 0.0183(2) 0.0162(2) 0.0167(2) -0.0010(2) -0.00100(14) -0.0016(2)
Cl2 0.079(4) 0.020(4) 0.041(3) 0.003(3) -0.028(3) -0.013(3)
P3 0.0152(5) 0.0182(5) 0.0181(5) -0.0022(4) 0.0009(4) -0.0011(4)
C4 0.022(2) 0.026(2) 0.030(2) 0.001(2) -0.004(2) 0.001(2)
C5 0.037(3) 0.037(3) 0.035(3) 0.000(2) -0.014(2) -0.001(3)
C6 0.033(3) 0.062(4) 0.048(3) -0.007(3) -0.009(2) 0.026(3)
C7 0.025(2) 0.025(2) 0.026(2) 0.002(2) 0.002(2) -0.006(2)
C8 0.031(3) 0.044(3) 0.039(3) -0.004(3) 0.016(2) -0.008(2)
C9 0.045(3) 0.031(3) 0.032(3) -0.001(2) 0.007(2) -0.017(2)
C10 0.020(2) 0.021(2) 0.019(2) -0.008(2) 0.002(2) -0.002(2)
C11 0.023(3) 0.036(3) 0.030(2) 0.000(2) 0.012(2) -0.002(2)
C12 0.022(2) 0.034(3) 0.035(3) -0.001(2) 0.001(2) 0.009(2)
N13 0.036(6) 0.021(9) 0.065(12) -0.026(7) -0.027(6) 0.010(6)
N14 0.076(9) 0.029(10) 0.050(11) 0.012(6) -0.020(8) -0.027(7)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.0000 0.0000 0.0000 0.01707(14) Uani 1 d S .
Cl2 Cl 0.0234(12) -0.1994(5) 0.0966(3) 0.0471(14) Uani 0.50 d P 1
P3 P 0.12429(12) 0.16589(11) 0.09669(6) 0.0171(2) Uani 1 d . .
C4 C 0.2693(5) 0.0716(5) 0.1709(3) 0.0264(9) Uani 1 d . .
H4 H 0.2085(45) 0.0100(46) 0.1923(21) 0.015(9) Uiso 1 d . .
C5 C 0.3435(7) 0.1661(6) 0.2386(3) 0.0369(11) Uani 1 d . .
H5A H 0.2627(52) 0.2171(47) 0.2664(24) 0.025(12) Uiso 1 d . .
H5B H 0.3980(45) 0.0995(44) 0.2816(23) 0.019(10) Uiso 1 d . .
H5C H 0.4114(58) 0.2368(57) 0.2226(27) 0.042(14) Uiso 1 d . .
C6 C 0.4047(6) -0.0168(8) 0.1287(3) 0.0479(14) Uani 1 d . .
H6A H 0.4918(68) 0.0502(62) 0.1113(30) 0.061(18) Uiso 1 d . .
H6B H 0.3629(62) -0.0733(57) 0.0821(32) 0.056(16) Uiso 1 d . .
H6C H 0.4688(54) -0.0819(50) 0.1678(26) 0.036(12) Uiso 1 d . .
C7 C 0.2312(5) 0.3282(5) 0.0512(2) 0.0252(9) Uani 1 d . .
H7 H 0.1485(45) 0.3662(42) 0.0177(21) 0.015(10) Uiso 1 d . .
C8 C 0.3680(7) 0.2814(7) -0.0050(3) 0.0377(12) Uani 1 d . .
H8A H 0.4519(58) 0.2530(53) 0.0284(27) 0.036(14) Uiso 1 d . .
H8B H 0.3482(58) 0.2003(60) -0.0380(30) 0.053(16) Uiso 1 d . .
H8C H 0.3933(61) 0.3610(63) -0.0384(30) 0.055(16) Uiso 1 d . .
C9 C 0.2921(7) 0.4529(5) 0.1069(3) 0.0358(12) Uani 1 d . .
H9A H 0.3956(58) 0.4190(52) 0.1353(27) 0.041(13) Uiso 1 d . .
H9B H 0.3267(61) 0.5410(57) 0.0780(29) 0.052(15) Uiso 1 d . .
H9C H 0.2064(64) 0.4798(61) 0.1463(31) 0.066(16) Uiso 1 d . .
C10 C -0.0325(5) 0.2557(4) 0.1607(2) 0.0200(9) Uani 1 d . .
H10 H 0.0179(42) 0.3095(39) 0.1961(21) 0.010 Uiso 1 d . .
C11 C -0.1345(6) 0.1373(6) 0.2035(3) 0.0295(10) Uani 1 d . .
H11A H -0.1972(59) 0.0765(55) 0.1705(28) 0.045(14) Uiso 1 d . .
H11B H -0.2137(48) 0.1895(46) 0.2362(24) 0.024(11) Uiso 1 d . .
H11C H -0.0638(61) 0.0811(60) 0.2342(29) 0.056(16) Uiso 1 d . .
C12 C -0.1483(6) 0.3599(6) 0.1120(3) 0.0303(10) Uani 1 d . .
H12A H -0.1956(49) 0.3092(47) 0.0726(25) 0.023(11) Uiso 1 d . .
H12B H -0.2396(49) 0.3928(43) 0.1424(22) 0.019(10) Uiso 1 d . .
H12C H -0.0858(54) 0.4409(51) 0.0924(25) 0.035(13) Uiso 1 d . .
N13 N 0.0039(21) 0.1475(15) -0.0778(10) 0.041(4) Uani 0.50 d P 2
N14 N -0.0017(28) 0.2411(20) -0.1207(11) 0.052(5) Uani 0.50 d P 2
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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
Cl2 Ru1 P3 89.29(13) . . ?
Cl2 Ru1 P3 90.71(13) . 3 ?
P3 Ru1 P3 180.0 . 3 ?
P3 Ru1 N13 90.8(5) . . ?
P3 Ru1 N13 89.2(5) 3 . ?
Ru1 P3 C4 113.73(14) . . ?
Ru1 P3 C7 113.37(13) . . ?
Ru1 P3 C10 112.42(13) . . ?
C4 P3 C7 109.6(2) . . ?
C4 P3 C10 103.5(2) . . ?
C7 P3 C10 103.3(2) . . ?
P3 C4 C5 117.4(3) . . ?
P3 C4 C6 111.3(3) . . ?
C5 C4 C6 111.3(4) . . ?
P3 C7 C8 113.0(3) . . ?
P3 C7 C9 117.7(3) . . ?
C8 C7 C9 110.7(4) . . ?
P3 C10 C11 110.8(3) . . ?
P3 C10 C12 111.7(3) . . ?
C11 C10 C12 110.1(4) . . ?
Ru1 N13 N14 174.7(20) . . ?
P3 C4 H4 102.9(26) . . ?
C5 C4 H4 105.8(26) . . ?
C6 C4 H4 107.2(28) . . ?
C4 C5 H5A 112.5(26) . . ?
C4 C5 H5B 110.2(21) . . ?
C4 C5 H5C 113.9(31) . . ?
H5A C5 H5B 103.0(32) . . ?
H5A C5 H5C 104.4(41) . . ?
H5B C5 H5C 112.2(37) . . ?
C4 C6 H6A 110.4(34) . . ?
C4 C6 H6B 113.8(29) . . ?
C4 C6 H6C 110.9(24) . . ?
H6A C6 H6B 108.0(41) . . ?
H6A C6 H6C 101.2(38) . . ?
H6B C6 H6C 111.8(36) . . ?
P3 C7 H7 101.7(23) . . ?
C8 C7 H7 104.4(23) . . ?
C9 C7 H7 108.0(24) . . ?
C7 C8 H8A 103.7(29) . . ?
C7 C8 H8B 118.0(30) . . ?
C7 C8 H8C 109.6(31) . . ?
H8A C8 H8B 104.9(43) . . ?
H8A C8 H8C 114.4(43) . . ?
H8B C8 H8C 106.3(42) . . ?
C7 C9 H9A 108.2(27) . . ?
C7 C9 H9B 112.6(28) . . ?
C7 C9 H9C 111.4(31) . . ?
H9A C9 H9B 103.6(41) . . ?
H9A C9 H9C 110.2(39) . . ?
H9B C9 H9C 110.4(42) . . ?
P3 C10 H10 109.1(24) . . ?
C11 C10 H10 108.3(24) . . ?
C12 C10 H10 106.7(24) . . ?
C10 C11 H11A 115.0(30) . . ?
C10 C11 H11B 107.6(23) . . ?
C10 C11 H11C 108.2(32) . . ?
H11A C11 H11B 105.5(37) . . ?
H11A C11 H11C 109.4(43) . . ?
H11B C11 H11C 111.1(38) . . ?
C10 C12 H12A 108.8(27) . . ?
C10 C12 H12B 111.7(23) . . ?
C10 C12 H12C 109.2(26) . . ?
H12A C12 H12B 103.9(34) . . ?
H12A C12 H12C 111.0(37) . . ?
H12B C12 H12C 112.1(34) . . ?
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 Cl2 2.396(4) . ?
Ru1 P3 2.3727(10) . ?
Ru1 P3 2.3727(10) 3 ?
Ru1 N13 1.84(2) . ?
P3 C4 1.860(4) . ?
P3 C7 1.855(4) . ?
P3 C10 1.856(4) . ?
C4 C5 1.508(6) . ?
C4 C6 1.530(6) . ?
C7 C8 1.523(6) . ?
C7 C9 1.515(6) . ?
C10 C11 1.527(6) . ?
C10 C12 1.522(6) . ?
N13 N14 1.10(2) . ?
C4 H4 0.82(4) . ?
C5 H5A 0.93(4) . ?
C5 H5B 1.01(4) . ?
C5 H5C 0.88(5) . ?
C6 H6A 0.97(5) . ?
C6 H6B 0.97(5) . ?
C6 H6C 1.00(5) . ?
C7 H7 0.91(4) . ?
C8 H8A 0.89(5) . ?
C8 H8B 0.92(5) . ?
C8 H8C 0.93(6) . ?
C9 H9A 0.98(5) . ?
C9 H9B 0.97(5) . ?
C9 H9C 1.00(5) . ?
C10 H10 0.85(3) . ?
C11 H11A 0.91(5) . ?
C11 H11B 0.97(4) . ?
C11 H11C 0.90(5) . ?
C12 H12A 0.87(4) . ?
C12 H12B 0.95(4) . ?
C12 H12C 0.94(5) . ?