#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/55/7205560.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_7205560
loop_
_publ_author_name
'Jipa, Ilona'
'Danova, Katya'
'Popovska, Nadejda'
'Siddiqi, M. Aslam'
'Siddiqui, Rehan A.'
'Atakan, Burak'
'Cremer, Till'
'Maier, Florian'
'Marbach, Hubertus'
'Steinrück, Hans-Peter'
'Heinemann, Frank W.'
'Zenneck, Ulrich'
_publ_section_title
;
 Methylated [(arene)(1,3-cyclohexadiene)Ru(0)] complexes as low-melting
 MOCVD precursor complexes with a controlled follow-up chemistry of the
 ligands
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              3014
_journal_paper_doi               10.1039/c0jm02652b
_journal_volume                  21
_journal_year                    2011
_chemical_formula_moiety         'C13 H16 Ru'
_chemical_formula_sum            'C13 H16 Ru'
_chemical_formula_weight         273.33
_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                91.821(3)
_cell_angle_beta                 108.474(4)
_cell_angle_gamma                93.874(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6694(4)
_cell_length_b                   8.2740(4)
_cell_length_c                   8.5494(2)
_cell_measurement_reflns_used    118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     512.57(4)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
ω-rotations with 2.00 ° and 70 sec per frame
;
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10165
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0231
_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)+(0.0216P)²+0.4239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                2187
_reflns_number_total             2438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0JM02652B.TXT
_cod_data_source_block           ij0605
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7205560
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 0.23420(3) 0.75090(2) 0.27183(2) 0.01518(7) Uani 1 1 d . . .
C1 C 0.2237(4) 0.6045(4) 0.4853(3) 0.0308(6) Uani 1 1 d . . .
H1A H 0.3181 0.5672 0.5752 0.037 Uiso 1 1 calc R . .
C2 C 0.1550(4) 0.7571(4) 0.4990(3) 0.0365(7) Uani 1 1 d . . .
H2A H 0.2081 0.8254 0.5964 0.044 Uiso 1 1 calc R . .
C3 C 0.0098(4) 0.8076(4) 0.3701(4) 0.0392(7) Uani 1 1 d . . .
H3A H -0.0363 0.9096 0.3809 0.047 Uiso 1 1 calc R . .
C4 C -0.0679(4) 0.7105(4) 0.2268(4) 0.0347(7) Uani 1 1 d . . .
H4A H -0.1684 0.7455 0.1409 0.042 Uiso 1 1 calc R . .
C5 C -0.0006(4) 0.5634(3) 0.2075(3) 0.0269(6) Uani 1 1 d . . .
H5A H -0.0549 0.4983 0.1080 0.032 Uiso 1 1 calc R . .
C6 C 0.1496(4) 0.5077(3) 0.3352(3) 0.0257(5) Uani 1 1 d . . .
C7 C 0.5099(3) 0.8239(3) 0.2860(3) 0.0229(5) Uani 1 1 d . . .
H7A H 0.6158 0.8177 0.3800 0.027 Uiso 1 1 calc R . .
C8 C 0.4420(3) 0.6961(3) 0.1594(3) 0.0205(5) Uani 1 1 d . . .
H8A H 0.4964 0.5899 0.1856 0.025 Uiso 1 1 calc R . .
C9 C 0.3913(3) 0.7389(3) -0.0203(3) 0.0206(5) Uani 1 1 d . . .
H9A H 0.3265 0.6431 -0.0928 0.025 Uiso 1 1 calc R . .
H9B H 0.5048 0.7703 -0.0474 0.025 Uiso 1 1 calc R . .
C10 C 0.2663(3) 0.8797(3) -0.0506(3) 0.0207(5) Uani 1 1 d . . .
H10A H 0.3189 0.9675 -0.1024 0.025 Uiso 1 1 calc R . .
H10B H 0.1427 0.8416 -0.1271 0.025 Uiso 1 1 calc R . .
C11 C 0.2490(3) 0.9448(3) 0.1116(3) 0.0202(5) Uani 1 1 d . . .
H11A H 0.1573 1.0274 0.1019 0.024 Uiso 1 1 calc R . .
C12 C 0.4039(4) 0.9609(3) 0.2579(3) 0.0223(5) Uani 1 1 d . . .
H12A H 0.4340 1.0552 0.3307 0.027 Uiso 1 1 calc R . .
C13 C 0.2226(5) 0.3499(4) 0.3088(5) 0.0444(8) Uani 1 1 d . . .
H13A H 0.1534 0.2616 0.3429 0.067 Uiso 1 1 calc R . .
H13B H 0.3533 0.3527 0.3745 0.067 Uiso 1 1 calc R . .
H13C H 0.2091 0.3319 0.1915 0.067 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'
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
C7 Ru1 C12 39.05(10) . . ?
C7 Ru1 C11 67.70(9) . . ?
C12 Ru1 C11 38.67(9) . . ?
C7 Ru1 C8 39.01(9) . . ?
C12 Ru1 C8 67.59(9) . . ?
C11 Ru1 C8 73.21(9) . . ?
C7 Ru1 C6 122.91(10) . . ?
C12 Ru1 C6 160.66(10) . . ?
C11 Ru1 C6 156.32(10) . . ?
C8 Ru1 C6 101.68(9) . . ?
C7 Ru1 C2 119.53(10) . . ?
C12 Ru1 C2 112.43(9) . . ?
C11 Ru1 C2 129.03(10) . . ?
C8 Ru1 C2 146.86(12) . . ?
C6 Ru1 C2 67.24(10) . . ?
C7 Ru1 C3 143.30(11) . . ?
C12 Ru1 C3 112.75(10) . . ?
C11 Ru1 C3 104.67(10) . . ?
C8 Ru1 C3 176.30(11) . . ?
C6 Ru1 C3 79.03(10) . . ?
C2 Ru1 C3 36.75(12) . . ?
C7 Ru1 C5 149.86(10) . . ?
C12 Ru1 C5 160.62(10) . . ?
C11 Ru1 C5 121.99(10) . . ?
C8 Ru1 C5 112.70(10) . . ?
C6 Ru1 C5 37.68(10) . . ?
C2 Ru1 C5 78.35(10) . . ?
C3 Ru1 C5 65.66(11) . . ?
C7 Ru1 C4 169.73(10) . . ?
C12 Ru1 C4 131.80(11) . . ?
C11 Ru1 C4 102.05(10) . . ?
C8 Ru1 C4 140.64(11) . . ?
C6 Ru1 C4 66.79(10) . . ?
C2 Ru1 C4 65.89(11) . . ?
C3 Ru1 C4 36.31(12) . . ?
C5 Ru1 C4 36.21(11) . . ?
C7 Ru1 C1 111.62(10) . . ?
C12 Ru1 C1 131.66(10) . . ?
C11 Ru1 C1 164.93(10) . . ?
C8 Ru1 C1 116.37(10) . . ?
C6 Ru1 C1 37.24(10) . . ?
C2 Ru1 C1 37.10(12) . . ?
C3 Ru1 C1 66.36(11) . . ?
C5 Ru1 C1 66.70(10) . . ?
C4 Ru1 C1 78.06(10) . . ?
C2 C1 C6 119.2(2) . . ?
C2 C1 Ru1 70.29(14) . . ?
C6 C1 Ru1 70.15(13) . . ?
C2 C1 H1A 120.4 . . ?
C6 C1 H1A 120.4 . . ?
Ru1 C1 H1A 131.9 . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 Ru1 71.63(15) . . ?
C1 C2 Ru1 72.61(14) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
Ru1 C2 H2A 128.0 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 Ru1 72.37(16) . . ?
C2 C3 Ru1 71.63(16) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
Ru1 C3 H3A 128.6 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 Ru1 71.41(15) . . ?
C3 C4 Ru1 71.32(16) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
Ru1 C4 H4A 130.1 . . ?
C4 C5 C6 120.8(2) . . ?
C4 C5 Ru1 72.38(16) . . ?
C6 C5 Ru1 71.05(14) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
Ru1 C5 H5A 129.4 . . ?
C1 C6 C5 118.5(2) . . ?
C1 C6 C13 122.0(3) . . ?
C5 C6 C13 119.5(3) . . ?
C1 C6 Ru1 72.61(14) . . ?
C5 C6 Ru1 71.27(14) . . ?
C13 C6 Ru1 127.88(18) . . ?
C12 C7 C8 113.7(2) . . ?
C12 C7 Ru1 70.68(14) . . ?
C8 C7 Ru1 72.23(13) . . ?
C12 C7 H7A 123.1 . . ?
C8 C7 H7A 123.1 . . ?
Ru1 C7 H7A 125.6 . . ?
C7 C8 C9 118.8(2) . . ?
C7 C8 Ru1 68.76(13) . . ?
C9 C8 Ru1 113.08(16) . . ?
C7 C8 H8A 115.9 . . ?
C9 C8 H8A 115.9 . . ?
Ru1 C8 H8A 115.9 . . ?
C8 C9 C10 109.97(19) . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C11 C10 C9 110.17(19) . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 Ru1 69.39(13) . . ?
C10 C11 Ru1 111.33(15) . . ?
C12 C11 H11A 115.6 . . ?
C10 C11 H11A 115.6 . . ?
Ru1 C11 H11A 115.6 . . ?
C11 C12 C7 114.3(2) . . ?
C11 C12 Ru1 71.94(13) . . ?
C7 C12 Ru1 70.26(13) . . ?
C11 C12 H12A 122.9 . . ?
C7 C12 H12A 122.9 . . ?
Ru1 C12 H12A 126.6 . . ?
C6 C13 H13A 109.5 . . ?
C6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
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 C7 2.124(2) . ?
Ru1 C12 2.129(2) . ?
Ru1 C11 2.163(2) . ?
Ru1 C8 2.170(2) . ?
Ru1 C6 2.209(2) . ?
Ru1 C2 2.211(2) . ?
Ru1 C3 2.211(3) . ?
Ru1 C5 2.212(2) . ?
Ru1 C4 2.225(3) . ?
Ru1 C1 2.242(2) . ?
C1 C2 1.417(4) . ?
C1 C6 1.422(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.394(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.382(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.379(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.428(4) . ?
C5 H5A 0.9500 . ?
C6 C13 1.493(4) . ?
C7 C12 1.421(4) . ?
C7 C8 1.434(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.521(3) . ?
C8 H8A 1.0000 . ?
C9 C10 1.535(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.520(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.421(4) . ?
C11 H11A 1.0000 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
