 
data_p21onm 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C11 H23 Cl2 N5 O3 Ru S' 
_chemical_formula_weight          477.37 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'  -0.0001   0.0005 
 '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'   0.0005   0.0010 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0017   0.0018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.0444   0.0408 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1495   0.1591 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ru'  'Ru'  -0.1866   2.2043 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/m
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x, -y-1/2, z' 
 
_cell_length_a                    9.313(2) 
_cell_length_b                    7.0555(14) 
_cell_length_c                    14.116(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  97.977(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      918.6(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     6707
_cell_measurement_theta_min       2.26
_cell_measurement_theta_max       14.92
 
_exptl_crystal_description        plate
_exptl_crystal_colour             'orange-yellow'
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.030
_exptl_crystal_size_min           0.005
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.726 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              484 
_exptl_absorpt_coefficient_mu     1.427 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5991  
_exptl_absorpt_correction_T_max   0.7439
_exptl_absorpt_process_details    
;
SADABS-2014/2 (Bruker, 2014/2) was used for the absorption 
correction. 
wR2(int) was 0.1101 and 0.0896 before and after correction
respectively. 
Ratio of minimum to maximum transmission is 0.8054.
;
 
_exptl_special_details 
; 
 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.41328 
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          
;
ChemMatCars beamline at the Advanced Photon Source,
Argonne National Laboratory, USA
; 
_diffrn_radiation_monochromator   'Silicon 111'
_diffrn_measurement_device_type  
; 
Bruker SMART APEX2 area detector
;
_diffrn_measurement_device        'three-circle diffractometer' 
_diffrn_measurement_method        'φ scans' 
_diffrn_detector_area_resol_mean  7.9
_diffrn_reflns_number             54860 
_diffrn_reflns_av_R_equivalents   0.1229 
_diffrn_reflns_av_sigmaI/netI     0.0488 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.63 
_diffrn_reflns_theta_max          15.61 
_reflns_number_total              2243 
_reflns_number_gt                 1898 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0798P)²+2.5710P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2243 
_refine_ls_number_parameters      143 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0656 
_refine_ls_R_factor_gt            0.0543 
_refine_ls_wR_factor_ref          0.1449 
_refine_ls_wR_factor_gt           0.1368 
_refine_ls_goodness_of_fit_ref    1.061 
_refine_ls_restrained_S_all       1.061 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 0.21038(5) 0.2500 0.87153(3) 0.02779(19) Uani 1 2 d S . . 
S1 S 0.27318(19) 0.2500 1.02161(13) 0.0297(6) Uani 0.917(8) 2 d SP A 1 
S1A S 0.313(3) 0.2500 1.093(2) 0.052(9) Uiso 0.083(8) 2 d SP A 2 
O1 O 0.1698(6) 0.2500 1.0891(4) 0.0387(11) Uani 1 2 d S . . 
O2 O 0.4218(6) 0.2500 1.0630(4) 0.0470(13) Uani 1 2 d S . . 
N1 N 0.0565(4) 0.0325(6) 0.8820(3) 0.0339(9) Uani 1 1 d . A . 
N3 N 0.3608(5) 0.0341(7) 0.8471(3) 0.0393(10) Uani 1 1 d . A . 
N5 N 0.1334(6) 0.2500 0.7232(4) 0.0283(11) Uani 1 2 d S A . 
C1 C -0.0104(8) 0.2500 0.6934(5) 0.0338(14) Uani 1 2 d S . . 
H1C H -0.0739 0.2500 0.7387 0.041 Uiso 1 2 calc SR A . 
C2 C -0.0653(8) 0.2500 0.5991(6) 0.0415(17) Uani 1 2 d S A . 
H2A H -0.1652 0.2500 0.5810 0.050 Uiso 1 2 calc SR . . 
C3 C 0.0263(9) 0.2500 0.5293(6) 0.0442(18) Uani 1 2 d S . . 
H3C H -0.0116 0.2500 0.4648 0.053 Uiso 1 2 calc SR A . 
C4 C 0.1747(8) 0.2500 0.5572(5) 0.0350(14) Uani 1 2 d S A . 
C5 C 0.2226(7) 0.2500 0.6547(5) 0.0286(13) Uani 1 2 d S . . 
H5A H 0.3221 0.2500 0.6745 0.034 Uiso 1 2 calc SR A . 
C6 C 0.2774(9) 0.2500 0.4864(5) 0.0415(17) Uani 1 2 d S . . 
C7 C 0.2376(11) 0.2500 0.3940(7) 0.098(6) Uani 1 2 d S A . 
H7A H 0.1388 0.2500 0.3720 0.118 Uiso 1 2 calc SR . . 
C8 C 0.3336(13) 0.2500 0.3253(7) 0.102(6) Uani 1 2 d S . . 
H8A H 0.2971 0.2500 0.2605 0.122 Uiso 1 2 calc SR A . 
C9 C 0.4718(10) 0.2500 0.3515(6) 0.052(2) Uani 1 2 d S . . 
H9A H 0.5379 0.2500 0.3031 0.062 Uiso 1 2 calc SR . . 
C10 C 0.5156(14) 0.1656(16) 0.4420(9) 0.108(4) Uani 1 1 d . . . 
C11 C 0.4221(12) 0.1633(15) 0.5131(8) 0.099(3) Uani 1 1 d . . . 
Cl1 Cl 0.2434(2) -0.2500 1.04794(14) 0.0456(5) Uani 1 2 d S . . 
Cl2 Cl -0.1480(2) 0.2500 0.28814(12) 0.0361(4) Uani 1 2 d S . . 
O1W O 0.3978(9) -0.2500 1.2534(7) 0.138(6) Uani 1 2 d S . . 
 
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 0.0341(3) 0.0213(3) 0.0275(3) 0.000 0.00231(18) 0.000 
S1 0.0301(10) 0.0274(10) 0.0308(12) 0.000 0.0011(7) 0.000 
O1 0.043(3) 0.036(3) 0.037(3) 0.000 0.006(2) 0.000 
O2 0.039(3) 0.048(3) 0.051(3) 0.000 -0.005(2) 0.000 
N1 0.040(2) 0.026(2) 0.036(2) 0.0004(16) 0.0087(17) -0.0060(16) 
N3 0.041(2) 0.031(2) 0.044(2) -0.0017(18) -0.0004(18) 0.0079(18) 
N5 0.029(3) 0.025(3) 0.030(3) 0.000 0.003(2) 0.000 
C1 0.038(4) 0.032(4) 0.033(3) 0.000 0.012(3) 0.000 
C2 0.030(3) 0.051(5) 0.041(4) 0.000 -0.002(3) 0.000 
C3 0.040(4) 0.058(5) 0.033(4) 0.000 -0.001(3) 0.000 
C4 0.036(3) 0.036(4) 0.034(4) 0.000 0.006(3) 0.000 
C5 0.029(3) 0.027(3) 0.029(3) 0.000 0.004(2) 0.000 
C6 0.042(4) 0.048(5) 0.034(4) 0.000 0.005(3) 0.000 
C7 0.037(5) 0.221(19) 0.037(5) 0.000 0.004(4) 0.000 
C8 0.061(6) 0.220(19) 0.026(5) 0.000 0.011(4) 0.000 
C9 0.058(5) 0.062(6) 0.040(4) 0.000 0.021(4) 0.000 
C10 0.134(9) 0.075(6) 0.128(9) -0.024(6) 0.058(7) -0.010(6) 
C11 0.117(8) 0.072(6) 0.110(8) -0.006(5) 0.027(6) 0.005(6) 
Cl1 0.0462(10) 0.0486(12) 0.0424(10) 0.000 0.0076(8) 0.000 
Cl2 0.0448(9) 0.0306(9) 0.0323(8) 0.000 0.0036(7) 0.000 
O1W 0.052(5) 0.299(19) 0.058(5) 0.000 -0.007(4) 0.000 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
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 N5 2.118(6) . ? 
Ru1 S1 2.118(2) . ? 
Ru1 N1 2.119(4) . ? 
Ru1 N1 2.119(4) 4_565 ? 
Ru1 N3 2.130(4) . ? 
Ru1 N3 2.130(4) 4_565 ? 
S1 O2 1.426(6) . ? 
S1 O1 1.446(6) . ? 
S1A O2 1.15(3) . ? 
S1A O1 1.33(3) . ? 
N5 C1 1.347(9) . ? 
N5 C5 1.359(8) . ? 
C1 C2 1.358(11) . ? 
C2 C3 1.390(11) . ? 
C3 C4 1.383(10) . ? 
C4 C5 1.387(10) . ? 
C4 C6 1.477(10) . ? 
C6 C7 1.305(13) . ? 
C6 C11 1.480(12) . ? 
C6 C11 1.480(12) 4_565 ? 
C7 C8 1.408(13) . ? 
C8 C9 1.289(14) . ? 
C9 C10 1.418(16) 4_565 ? 
C9 C10 1.418(16) . ? 
C10 C10 1.19(2) 4_565 ? 
C10 C11 1.416(14) . ? 
C10 C11 1.861(14) 4_565 ? 
C11 C11 1.22(2) 4_565 ? 
C11 C10 1.861(14) 4_565 ? 
 
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 
N5 Ru1 S1 176.27(15) . . ? 
N5 Ru1 N1 85.95(15) . . ? 
S1 Ru1 N1 91.48(12) . . ? 
N5 Ru1 N1 85.95(15) . 4_565 ? 
S1 Ru1 N1 91.48(12) . 4_565 ? 
N1 Ru1 N1 92.8(2) . 4_565 ? 
N5 Ru1 N3 88.86(16) . . ? 
S1 Ru1 N3 93.74(13) . . ? 
N1 Ru1 N3 87.68(18) . . ? 
N1 Ru1 N3 174.74(16) 4_565 . ? 
N5 Ru1 N3 88.86(16) . 4_565 ? 
S1 Ru1 N3 93.74(13) . 4_565 ? 
N1 Ru1 N3 174.74(16) . 4_565 ? 
N1 Ru1 N3 87.68(18) 4_565 4_565 ? 
N3 Ru1 N3 91.4(3) . 4_565 ? 
O2 S1 O1 115.3(4) . . ? 
O2 S1 Ru1 121.9(3) . . ? 
O1 S1 Ru1 122.9(2) . . ? 
O2 S1A O1 156(3) . . ? 
S1A O1 S1 43.0(14) . . ? 
S1A O2 S1 45.2(16) . . ? 
C1 N5 C5 117.2(6) . . ? 
C1 N5 Ru1 119.6(4) . . ? 
C5 N5 Ru1 123.2(4) . . ? 
N5 C1 C2 121.9(6) . . ? 
C1 C2 C3 120.7(7) . . ? 
C4 C3 C2 119.0(7) . . ? 
C3 C4 C5 117.0(7) . . ? 
C3 C4 C6 121.5(7) . . ? 
C5 C4 C6 121.5(6) . . ? 
N5 C5 C4 124.2(6) . . ? 
C7 C6 C4 123.7(8) . . ? 
C7 C6 C11 112.1(8) . . ? 
C4 C6 C11 118.7(7) . . ? 
C7 C6 C11 112.1(8) . 4_565 ? 
C4 C6 C11 118.7(7) . 4_565 ? 
C11 C6 C11 48.8(9) . 4_565 ? 
C6 C7 C8 124.7(10) . . ? 
C9 C8 C7 120.4(9) . . ? 
C8 C9 C10 114.2(8) . 4_565 ? 
C8 C9 C10 114.2(8) . . ? 
C10 C9 C10 49.7(9) 4_565 . ? 
C10 C10 C11 90.6(6) 4_565 . ? 
C10 C10 C9 65.2(5) 4_565 . ? 
C11 C10 C9 121.0(11) . . ? 
C10 C10 C11 49.6(5) 4_565 4_565 ? 
C11 C10 C11 41.1(8) . 4_565 ? 
C9 C10 C11 96.7(8) . 4_565 ? 
C11 C11 C10 89.4(6) 4_565 . ? 
C11 C11 C6 65.6(4) 4_565 . ? 
C10 C11 C6 116.2(11) . . ? 
C11 C11 C10 49.6(5) 4_565 4_565 ? 
C10 C11 C10 39.8(8) . 4_565 ? 
C6 C11 C10 94.1(8) . 4_565 ? 
 
_diffrn_measured_fraction_theta_max    0.976 
_diffrn_reflns_theta_full              15.61 
_diffrn_measured_fraction_theta_full   0.976 
_refine_diff_density_max    1.129 
_refine_diff_density_min   -1.438 
_refine_diff_density_rms    0.162 

# start Validation Reply Form
_vrf_RINTA01_p21onm
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: This structure appears to be a pseudo-merehedral twin in P2(1)
rather than this P2(1)/m model which is shown here for comparison. A
high Rint is characteristic of a pseudo-merehedral twin.
;
_vrf_PLAT029_p21onm
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.976 Why?  
RESPONSE: this is from light induced in situ diffraction data collected
at a synchrotron, where not all angles could be accessed owing to 
physical obstructions such as the LED light and fiber optics, detector,
in house cryostream, synchrotron beam optics limitations. Moreover, the 
experiment was time limited. Thus, the data coverage is slightly 
compromised but it is nonetheless still good full coverage of 98%.
;
_vrf_PLAT043_p21onm
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       7.90 Check 
RESPONSE: 8 H atoms could not be observed or modelled.
;
_vrf_PLAT230_p21onm
;
PROBLEM: Hirshfeld Test Diff for    C6       --C11      .        7.3 s.u.  
RESPONSE: There is heavy disorder in the phenyl group to which C6 and 
C11 belong. Moreover, this disorder is disrupting
the mirror plane of this space group, P2(1)/m, associated with this model
which appears to really be a pseudo-merehedral twin in P2(1).
;
_vrf_PLAT306_p21onm
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: O1W is the oxygen of a water molecule. Its H atoms could not
be observed or modelled and so it appears as an isolated atom.
;
_vrf_PLAT362_p21onm
;
PROBLEM: Short  C(sp3)-C(sp2) Bond  C6       - C7       .       1.31 Ang.  
RESPONSE: There is heavy disorder in the phenyl group to which C6 and 
C7 belong. Moreover, this disorder is disrupting
the mirror plane of this space group, P2(1)/m, associated with this model
which appears to really be a pseudo-merehedral twin in P2(1).
;
_vrf_PLAT041_p21onm
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: 8 H atoms could not be observed or modelled.
;
_vrf_PLAT220_p21onm
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.9 Ratio 
RESPONSE: There is heavy disorder in the phenyl group which is disrupting
the mirror plane of this space group, P2(1)/m. The ADPs are trying to 
compensate.
;
_vrf_PLAT241_p21onm
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C7 Check 
RESPONSE: There is heavy disorder in the phenyl group which is disrupting
the mirror plane of this space group, P2(1)/m. The ADPs are trying to 
compensate.
;
_vrf_PLAT242_p21onm
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C6 Check 
RESPONSE: There is heavy disorder in the phenyl group which is disrupting
the mirror plane of this space group, P2(1)/m. The ADPs are trying to 
compensate.
;
_vrf_PLAT260_p21onm
;
PROBLEM: Large Average Ueq of Residue Including       O1W      0.138 Check 
RESPONSE: This the water molecule trying to stay in the mirror plane of 
this space group, P2(1)/m. The ADPs are trying to compensate.
;
_vrf_PLAT342_p21onm
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01353 Ang.  
RESPONSE: There is heavy disorder in the phenyl group which comprise 
over half of the total number of carbon atoms (and thus bonds) in this
crystal structure. Thus, the average precision of C-C bonds is low.
;
_vrf_PLAT911_p21onm
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         32 Report
RESPONSE: Some reflections were removed owing to extinction effects.
;
_vrf_PLAT975_p21onm
;
PROBLEM: Check Calcd Resid. Dens.  1.00A   From N3              0.64 eA-3  
RESPONSE: Checked but not due to a H.
;
_vrf_PLAT976_p21onm
;
PROBLEM: Check Calcd Resid. Dens.  0.45A   From O1W            -0.61 eA-3  
RESPONSE: Checked but not due to a H.
;
_vrf_PLAT977_p21onm
;
PROBLEM: Check Negative Difference Density on H8A              -0.33 eA-3  
RESPONSE: There is heavy disorder in the phenyl group to which this H8A
is attached, so it is proving hard to model it as a riding atom when 
the adjoining carbon is ill-defined.
;
# end Validation Reply Form
