#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:17:46 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177770 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/78/7037806.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_7037806
loop_
_publ_author_name
'Ferrer, Íngrid'
'Fontrodona, Xavier'
'Rodríguez, Montserrat'
'Romero, Isabel'
_publ_section_title
;
 Ru(ii)-dmso complexes containing azole-based ligands: synthesis, linkage
 isomerism and catalytic behaviour.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3163
_journal_page_last               3174
_journal_paper_doi               10.1039/c5dt04376j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C13 H23 Br Cl2 N2 O3 Ru S3, O H2'
_chemical_formula_sum            'C13 H25 Br Cl2 N2 O4 Ru S3'
_chemical_formula_weight         621.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.27(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.493(6)
_cell_length_b                   13.943(7)
_cell_length_c                   16.522(6)
_cell_measurement_reflns_used    4395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.18
_cell_volume                     2195.9(18)
_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  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.824626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5402
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0503P)²+2.9706P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4341
_reflns_number_total             5402
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04376j2.cif
_cod_data_source_block           complex4bgrocs
_cod_depositor_comments
'Adding full bibliography for 7037805--7037809.cif.'
_cod_database_code               7037806
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ru1 Ru 0.79518(3) 0.17111(2) 0.70012(2) 0.03145(9) Uani 1 1 d . .
Br1 Br 0.66884(6) -0.40099(4) 0.77703(5) 0.07351(18) Uani 1 1 d . .
S1 S 1.02961(10) 0.15983(7) 0.83977(7) 0.0420(2) Uani 1 1 d . U
C1 C 0.7311(4) -0.1165(3) 0.7556(3) 0.0392(8) Uani 1 1 d . .
N1 N 0.7510(3) 0.0407(2) 0.7418(2) 0.0381(7) Uani 1 1 d . .
O1 O 1.1221(3) 0.1292(3) 0.8204(3) 0.0736(10) Uani 1 1 d . U
Cl1 Cl 0.77391(12) 0.24767(8) 0.82069(9) 0.0537(3) Uani 1 1 d . .
N2 N 0.7893(3) -0.0488(2) 0.7365(3) 0.0423(7) Uani 1 1 d . .
H2B H 0.8436 -0.0607 0.7227 0.051 Uiso 1 1 calc R U
C2 C 0.7390(4) -0.2168(3) 0.7550(3) 0.0463(9) Uani 1 1 d . .
H2A H 0.7907 -0.2484 0.7407 0.056 Uiso 1 1 calc R U
S2 S 0.82017(10) 0.31495(7) 0.64810(8) 0.0422(2) Uani 1 1 d . .
Cl2 Cl 0.54318(10) 0.18330(8) 0.56188(8) 0.0504(2) Uani 1 1 d . .
O2 O 0.9583(3) 0.3358(2) 0.6791(3) 0.0566(8) Uani 1 1 d . .
S3 S 0.82225(10) 0.08252(7) 0.59766(8) 0.0423(2) Uani 1 1 d . U
C3 C 0.6657(4) -0.2643(3) 0.7769(3) 0.0465(9) Uani 1 1 d . .
O3 O 0.8888(5) -0.0080(3) 0.6384(4) 0.0873(12) Uani 1 1 d . U
C4 C 0.5867(4) -0.2200(3) 0.7988(3) 0.0483(10) Uani 1 1 d . .
H4A H 0.5393 -0.2570 0.8136 0.058 Uiso 1 1 calc R U
C5 C 0.5791(4) -0.1219(3) 0.7983(3) 0.0466(9) Uani 1 1 d . .
H5A H 0.5265 -0.0915 0.8125 0.056 Uiso 1 1 calc R U
C6 C 0.6529(4) -0.0682(3) 0.7758(3) 0.0366(8) Uani 1 1 d . .
C7 C 0.6697(4) 0.0301(3) 0.7655(3) 0.0417(8) Uani 1 1 d . .
H7A H 0.6289 0.0802 0.7742 0.050 Uiso 1 1 calc R U
C8 C 1.1052(5) 0.2667(3) 0.9179(4) 0.0603(12) Uani 1 1 d . .
H8A H 1.2036 0.2568 0.9752 0.090 Uiso 1 1 calc R U
H8B H 1.0601 0.2820 0.9462 0.090 Uiso 1 1 calc R U
H8C H 1.0926 0.3187 0.8743 0.090 Uiso 1 1 calc R U
C9 C 1.0604(5) 0.0797(4) 0.9367(4) 0.0722(15) Uani 1 1 d . .
H9A H 1.1593 0.0755 0.9952 0.108 Uiso 1 1 calc R U
H9B H 1.0246 0.0174 0.9057 0.108 Uiso 1 1 calc R U
H9C H 1.0137 0.1031 0.9615 0.108 Uiso 1 1 calc R U
C10 C 0.6942(6) 0.3362(4) 0.5084(4) 0.0686(14) Uani 1 1 d . .
H10A H 0.7112 0.3978 0.4926 0.103 Uiso 1 1 calc R U
H10B H 0.6015 0.3350 0.4858 0.103 Uiso 1 1 calc R U
H10C H 0.7021 0.2872 0.4717 0.103 Uiso 1 1 calc R U
C11 C 0.7787(6) 0.4137(3) 0.6915(4) 0.0647(13) Uani 1 1 d . .
H11A H 0.7906 0.4724 0.6678 0.097 Uiso 1 1 calc R U
H11B H 0.8400 0.4136 0.7676 0.097 Uiso 1 1 calc R U
H11C H 0.6832 0.4084 0.6626 0.097 Uiso 1 1 calc R U
C12 C 0.9232(6) 0.1340(4) 0.5672(4) 0.0669(13) Uani 1 1 d . .
H12A H 0.9266 0.0903 0.5240 0.100 Uiso 1 1 calc R U
H12B H 1.0167 0.1464 0.6318 0.100 Uiso 1 1 calc R U
H12C H 0.8806 0.1931 0.5294 0.100 Uiso 1 1 calc R U
C13 C 0.6610(6) 0.0573(5) 0.4691(4) 0.090(2) Uani 1 1 d . .
H13A H 0.6789 0.0204 0.4299 0.136 Uiso 1 1 calc R U
H13B H 0.6158 0.1164 0.4325 0.136 Uiso 1 1 calc R U
H13C H 0.6011 0.0215 0.4755 0.136 Uiso 1 1 calc R U
O1W O 0.4156(7) 0.4030(6) 0.4991(6) 0.177(3) Uani 1 1 d . .
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'
Ru Ru -1.2594 0.8363 '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'
Br Br -0.2901 2.4595 '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
N1 Ru1 S1 92.62(9)
N1 Ru1 S2 174.28(8)
S1 Ru1 S2 92.45(4)
N1 Ru1 S3 88.37(9)
S1 Ru1 S3 90.23(5)
S2 Ru1 S3 94.25(5)
N1 Ru1 Cl2 85.09(9)
S1 Ru1 Cl2 175.43(4)
S2 Ru1 Cl2 89.66(4)
S3 Ru1 Cl2 93.66(5)
N1 Ru1 Cl1 85.50(9)
S1 Ru1 Cl1 87.14(5)
S2 Ru1 Cl1 92.11(5)
S3 Ru1 Cl1 173.21(4)
Cl2 Ru1 Cl1 88.73(5)
O1 S1 C9 105.9(3)
O1 S1 C8 106.3(2)
C9 S1 C8 99.6(3)
O1 S1 Ru1 118.91(16)
C9 S1 Ru1 110.07(17)
C8 S1 Ru1 114.00(16)
N2 C1 C6 106.6(3)
N2 C1 C2 130.3(4)
C6 C1 C2 123.1(3)
C7 N1 N2 106.8(3)
C7 N1 Ru1 127.0(3)
N2 N1 Ru1 125.8(2)
C1 N2 N1 111.3(3)
C1 N2 H2B 124.4
N1 N2 H2B 124.4
C3 C2 C1 115.1(4)
C3 C2 H2A 122.4
C1 C2 H2A 122.4
O2 S2 C11 106.8(2)
O2 S2 C10 105.7(2)
C11 S2 C10 98.6(3)
O2 S2 Ru1 117.12(13)
C11 S2 Ru1 112.47(17)
C10 S2 Ru1 114.28(18)
O3 S3 C13 104.8(3)
O3 S3 C12 100.8(3)
C13 S3 C12 101.8(3)
O3 S3 Ru1 116.77(17)
C13 S3 Ru1 113.25(19)
C12 S3 Ru1 117.43(18)
C2 C3 C4 124.4(4)
C2 C3 Br1 118.2(3)
C4 C3 Br1 117.4(3)
C5 C4 C3 120.0(4)
C5 C4 H4A 120.0
C3 C4 H4A 120.0
C4 C5 C6 118.4(4)
C4 C5 H5A 120.8
C6 C5 H5A 120.8
C1 C6 C5 119.1(4)
C1 C6 C7 104.9(3)
C5 C6 C7 136.1(4)
N1 C7 C6 110.5(3)
N1 C7 H7A 124.8
C6 C7 H7A 124.8
S1 C8 H8A 109.5
S1 C8 H8B 109.5
H8A C8 H8B 109.5
S1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
S1 C9 H9A 109.5
S1 C9 H9B 109.5
H9A C9 H9B 109.5
S1 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
S2 C10 H10A 109.5
S2 C10 H10B 109.5
H10A C10 H10B 109.5
S2 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
S2 C11 H11A 109.5
S2 C11 H11B 109.5
H11A C11 H11B 109.5
S2 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
S3 C12 H12A 109.5
S3 C12 H12B 109.5
H12A C12 H12B 109.5
S3 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
S3 C13 H13A 109.5
S3 C13 H13B 109.5
H13A C13 H13B 109.5
S3 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
Ru1 N1 2.140(3)
Ru1 S1 2.2782(15)
Ru1 S2 2.2816(14)
Ru1 S3 2.2904(11)
Ru1 Cl2 2.4210(16)
Ru1 Cl1 2.4213(12)
Br1 C3 1.906(5)
S1 O1 1.448(4)
S1 C9 1.779(5)
S1 C8 1.790(4)
C1 N2 1.347(4)
C1 C6 1.395(5)
C1 C2 1.402(6)
N1 C7 1.311(5)
N1 N2 1.359(4)
N2 H2B 0.8600
C2 C3 1.355(5)
C2 H2A 0.9300
S2 O2 1.478(3)
S2 C11 1.777(5)
S2 C10 1.788(5)
S3 O3 1.419(4)
S3 C13 1.778(5)
S3 C12 1.783(5)
C3 C4 1.395(6)
C4 C5 1.371(6)
C4 H4A 0.9300
C5 C6 1.411(5)
C5 H5A 0.9300
C6 C7 1.414(6)
C7 H7A 0.9300
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C9 H9A 0.9600
C9 H9B 0.9600
C9 H9C 0.9600
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
C11 H11A 0.9600
C11 H11B 0.9600
C11 H11C 0.9600
C12 H12A 0.9600
C12 H12B 0.9600
C12 H12C 0.9600
C13 H13A 0.9600
C13 H13B 0.9600
C13 H13C 0.9600
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
C6 C1 N2 N1 -0.9(4)
C2 C1 N2 N1 177.9(4)
C7 N1 N2 C1 0.7(4)
Ru1 N1 N2 C1 -172.4(2)
N2 C1 C2 C3 -179.3(4)
C6 C1 C2 C3 -0.7(6)
C1 C2 C3 C4 0.0(6)
C1 C2 C3 Br1 179.6(3)
C2 C3 C4 C5 0.4(6)
Br1 C3 C4 C5 -179.1(3)
C3 C4 C5 C6 -0.2(6)
N2 C1 C6 C5 179.8(3)
C2 C1 C6 C5 0.9(6)
N2 C1 C6 C7 0.7(4)
C2 C1 C6 C7 -178.2(4)
C4 C5 C6 C1 -0.4(6)
C4 C5 C6 C7 178.3(4)
N2 N1 C7 C6 -0.2(4)
Ru1 N1 C7 C6 172.8(2)
C1 C6 C7 N1 -0.3(4)
C5 C6 C7 N1 -179.1(4)
