#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/53/4065323.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_4065323
loop_
_publ_author_name
'Marchetti, Fabio'
'Pettinari, Claudio'
'Pettinari, Riccardo'
'Cerquetella, Adele'
'Martins, Luísa M. D. R. S.'
'Guedes da Silva, M. Fátima C.'
'Silva, Telma F. S.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Ruthenium(II) Arene Complexes Bearing Tris(pyrazolyl)methanesulfonate
 Capping Ligands. Electrochemistry, Spectroscopic, and X-ray Structural
 Characterization
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6180
_journal_paper_doi               10.1021/om200713v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C22 H27 N6 O3 Ru S, Cl'
_chemical_formula_sum            'C22 H27 Cl N6 O3 Ru S'
_chemical_formula_weight         592.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           164
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.115
_cell_length_b                   12.115
_cell_length_c                   10.3377(9)
_cell_measurement_reflns_used    1856
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.77
_cell_volume                     1314.02(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4445
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.8676
_exptl_absorpt_correction_T_min  0.7887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         3.644
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         929
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0698P)²+3.4644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                799
_reflns_number_total             929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200713v_si_001.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_database_code               4065323
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, 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
C1 C 0.8058(3) 0.6116(6) 0.4730(5) 0.0253(14) Uani 1 2 d S
H1 H 0.8275 0.6549 0.3923 0.030 Uiso 1 2 calc SR
C2 C 0.7884(3) 0.5768(6) 0.6818(5) 0.0215(13) Uani 1 2 d S
H2 H 0.7934 0.5868 0.7731 0.026 Uiso 1 2 calc SR
C3 C 0.8362(3) 0.6724(6) 0.5928(6) 0.0283(14) Uani 1 2 d S
H3 H 0.8808 0.7616 0.6089 0.034 Uiso 1 2 calc SR
C4 C 0.7845(4) 0.3336(4) 0.1852(3) 0.0231(10) Uani 1 1 d .
C5 C 0.9097(5) 0.3364(5) 0.1778(4) 0.0341(12) Uani 1 1 d .
H5A H 0.9472 0.3658 0.0919 0.051 Uiso 1 1 calc R
H5B H 0.8959 0.2506 0.1930 0.051 Uiso 1 1 calc R
H5C H 0.9677 0.3947 0.2437 0.051 Uiso 1 1 calc R
C10 C 0.6667 0.3333 0.6646(10) 0.0288(4) Uani 1 6 d SU
N1 N 0.7430(3) 0.4860(5) 0.4853(4) 0.0224(11) Uani 1 2 d S
N2 N 0.7322(2) 0.4644(5) 0.6165(4) 0.0196(11) Uani 1 2 d S
O1 O 0.8006(4) 0.4003(2) 0.8784(4) 0.0289(11) Uani 1 2 d S
S1 S 0.6667 0.3333 0.8493(2) 0.0213(6) Uani 1 6 d S
Ru1 Ru 0.6667 0.3333 0.35233(7) 0.0169(3) Uani 1 6 d S
Cl1 Cl 0.0000 0.0000 0.7118(3) 0.0538(10) Uani 1 6 d S
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 C1 C3 111.8(5) . .
N1 C1 H1 124.1 . .
C3 C1 H1 124.1 . .
N2 C2 C3 107.7(5) . .
N2 C2 H2 126.1 . .
C3 C2 H2 126.1 . .
C2 C3 C1 105.2(6) . .
C2 C3 H3 127.4 . .
C1 C3 H3 127.4 . .
C4 C4 C4 120.000(2) 11 12_665
C4 C4 C5 118.8(3) 11 .
C4 C4 C5 121.1(3) 12_665 .
C4 C4 Ru1 71.51(11) 11 .
C4 C4 Ru1 71.38(11) 12_665 .
C5 C4 Ru1 132.4(3) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C10 N2 109.1(4) 2_655 .
N2 C10 N2 109.1(4) 2_655 3_665
N2 C10 N2 109.1(4) . 3_665
N2 C10 S1 109.9(4) 2_655 .
N2 C10 S1 109.9(4) . .
N2 C10 S1 109.9(4) 3_665 .
C1 N1 N2 105.0(5) . .
C1 N1 Ru1 133.8(4) . .
N2 N1 Ru1 121.2(4) . .
C2 N2 N1 110.3(5) . .
C2 N2 C10 130.3(6) . .
N1 N2 C10 119.3(6) . .
O1 S1 O1 115.74(12) 3_665 2_655
O1 S1 O1 115.74(12) 3_665 .
O1 S1 O1 115.74(12) 2_655 .
O1 S1 C10 102.09(17) 3_665 .
O1 S1 C10 102.09(17) 2_655 .
O1 S1 C10 102.09(17) . .
N1 Ru1 N1 82.2(2) 3_665 2_655
N1 Ru1 N1 82.2(2) 3_665 .
N1 Ru1 N1 82.2(2) 2_655 .
N1 Ru1 C4 94.84(17) 3_665 .
N1 Ru1 C4 157.08(14) 2_655 .
N1 Ru1 C4 120.09(15) . .
N1 Ru1 C4 94.84(17) 3_665 12_665
N1 Ru1 C4 120.09(15) 2_655 12_665
N1 Ru1 C4 157.08(14) . 12_665
C4 Ru1 C4 37.2(2) . 12_665
N1 Ru1 C4 120.09(14) 3_665 3_665
N1 Ru1 C4 94.84(17) 2_655 3_665
N1 Ru1 C4 157.08(14) . 3_665
C4 Ru1 C4 66.91(17) . 3_665
C4 Ru1 C4 37.0(2) 12_665 3_665
N1 Ru1 C4 120.09(15) 3_665 11
N1 Ru1 C4 157.08(14) 2_655 11
N1 Ru1 C4 94.84(17) . 11
C4 Ru1 C4 37.0(2) . 11
C4 Ru1 C4 66.90(17) 12_665 11
C4 Ru1 C4 79.1(2) 3_665 11
N1 Ru1 C4 157.08(14) 3_665 10_655
N1 Ru1 C4 94.84(17) 2_655 10_655
N1 Ru1 C4 120.09(14) . 10_655
C4 Ru1 C4 79.1(2) . 10_655
C4 Ru1 C4 66.90(17) 12_665 10_655
C4 Ru1 C4 37.2(2) 3_665 10_655
C4 Ru1 C4 66.90(17) 11 10_655
N1 Ru1 C4 157.08(14) 3_665 2_655
N1 Ru1 C4 120.09(14) 2_655 2_655
N1 Ru1 C4 94.84(17) . 2_655
C4 Ru1 C4 66.91(17) . 2_655
C4 Ru1 C4 79.1(2) 12_665 2_655
C4 Ru1 C4 66.90(17) 3_665 2_655
C4 Ru1 C4 37.2(2) 11 2_655
C4 Ru1 C4 37.0(2) 10_655 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.324(8) .
C1 C3 1.393(8) .
C1 H1 0.9500 .
C2 N2 1.358(8) .
C2 C3 1.361(9) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 C4 1.422(9) 11
C4 C4 1.431(9) 12_665
C4 C5 1.502(6) .
C4 Ru1 2.241(4) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C10 N2 1.463(6) 2_655
C10 N2 1.463(6) .
C10 N2 1.463(6) 3_665
C10 S1 1.910(11) .
N1 N2 1.375(6) .
N1 Ru1 2.111(5) .
O1 S1 1.437(5) .
S1 O1 1.437(5) 3_665
S1 O1 1.437(5) 2_655
Ru1 N1 2.111(5) 3_665
Ru1 N1 2.111(5) 2_655
Ru1 C4 2.241(4) 12_665
Ru1 C4 2.241(4) 3_665
Ru1 C4 2.241(4) 11
Ru1 C4 2.241(4) 10_655
Ru1 C4 2.241(4) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 133.6 54.3
2 0.000 0.500 0.500 15.5 -0.4
3 0.500 0.500 0.500 15.3 -0.4
4 0.500 1.000 0.500 15.5 -0.4
