# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_art002_1
_database_code_depnum_ccdc_archive 'CCDC 1546164'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 N8 O11 Ru2'
_chemical_formula_sum            'C12 H14 N8 O11 Ru2'
_chemical_formula_weight         648.45

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.5957(5)
_cell_length_b                   14.4379(4)
_cell_length_c                   8.6771(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.4510(10)
_cell_angle_gamma                90
_cell_volume                     2153.08(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3919
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.45

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.475
_shelx_estimated_absorpt_T_min   0.809
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9851
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.370
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2472
_reflns_number_gt                2038
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond 3.2k'
_computing_publication_material  'Diamond 3.2k'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+0.0289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2472
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0492
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.41228(2) 0.18593(2) 0.11996(2) 0.02698(7) Uani 1 1 d . . . . .
O3 O 0.36155(12) 0.34856(14) 0.2409(2) 0.0567(5) Uani 1 1 d . . . . .
N4 N 0.39826(11) 0.27452(13) -0.0856(2) 0.0328(4) Uani 1 1 d . . . . .
N6 N 0.34253(11) 0.26878(15) 0.1969(2) 0.0364(5) Uani 1 1 d . . . . .
C10 C 0.41625(16) 0.36406(18) -0.0474(3) 0.0454(6) Uani 1 1 d . . . . .
H10 H 0.436735 0.381430 0.066867 0.054 Uiso 1 1 calc R U . . .
O11 O 0.28311(11) 0.23642(15) 0.2037(2) 0.0598(5) Uani 1 1 d . . . . .
C12 C 0.37193(15) 0.2492(2) -0.2481(3) 0.0462(6) Uani 1 1 d . . . . .
C13 C 0.40664(19) 0.4311(2) -0.1639(4) 0.0638(8) Uani 1 1 d . . . . .
H13 H 0.419832 0.493686 -0.131847 0.077 Uiso 1 1 calc R U . . .
C14 C 0.3622(2) 0.3163(2) -0.3677(4) 0.0661(9) Uani 1 1 d . . . . .
H14 H 0.344067 0.298493 -0.481685 0.079 Uiso 1 1 calc R U . . .
C16 C 0.35286(19) 0.1507(2) -0.2970(3) 0.0638(9) Uani 1 1 d . . . . .
H16A H 0.395624 0.111059 -0.227099 0.096 Uiso 1 1 calc R U . . .
H16B H 0.345407 0.142723 -0.414303 0.096 Uiso 1 1 calc R U . . .
H16C H 0.304973 0.133578 -0.281957 0.096 Uiso 1 1 calc R U . . .
C18 C 0.3776(2) 0.4060(3) -0.3277(4) 0.0765(10) Uani 1 1 d . . . . .
H18 H 0.368394 0.451377 -0.412400 0.092 Uiso 1 1 calc R U . . .
O1 O 0.500000 0.25805(14) 0.250000 0.0269(4) Uani 1 2 d S T P . .
O2 O 0.49219(9) 0.10825(11) 0.05503(19) 0.0393(4) Uani 1 1 d . . . . .
O4 O 0.39020(10) 0.06488(13) 0.3687(2) 0.0522(5) Uani 1 1 d . . . . .
N3 N 0.43759(11) 0.10949(13) 0.3361(2) 0.0347(4) Uani 1 1 d . . . . .
N5 N 0.33231(11) 0.11017(14) 0.0209(2) 0.0376(5) Uani 1 1 d . . . . .
O5 O 0.28509(11) 0.05533(14) -0.0174(3) 0.0635(5) Uani 1 1 d . . . . .


_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 1.781(2) . ?
Ru1 O1 1.9006(11) . ?
Ru1 N6 2.054(2) . ?
Ru1 N3 2.0696(19) . ?
Ru1 O2 2.1030(15) . ?
Ru1 N4 2.1284(18) . ?
O3 N6 1.222(3) . ?
N4 C10 1.345(3) . ?
N4 C12 1.354(3) . ?
N6 O11 1.222(3) . ?
C10 C13 1.361(3) . ?
C10 H10 0.9500 . ?
C12 C14 1.380(4) . ?
C12 C16 1.487(4) . ?
C13 C18 1.362(4) . ?
C13 H13 0.9500 . ?
C14 C18 1.344(4) . ?
C14 H14 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18 0.9500 . ?
O2 N3 1.287(2) 2_655 ?
O4 N3 1.209(2) . ?
N5 O5 1.134(2) . ?

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 O1 172.91(7) . . ?
N5 Ru1 N6 90.00(9) . . ?
O1 Ru1 N6 89.62(7) . . ?
N5 Ru1 N3 88.21(8) . . ?
O1 Ru1 N3 84.70(6) . . ?
N6 Ru1 N3 88.25(7) . . ?
N5 Ru1 O2 95.07(7) . . ?
O1 Ru1 O2 85.25(5) . . ?
N6 Ru1 O2 174.87(7) . . ?
N3 Ru1 O2 91.09(7) . . ?
N5 Ru1 N4 98.75(8) . . ?
O1 Ru1 N4 88.34(6) . . ?
N6 Ru1 N4 91.82(7) . . ?
N3 Ru1 N4 173.04(7) . . ?
O2 Ru1 N4 88.22(7) . . ?
C10 N4 C12 118.2(2) . . ?
C10 N4 Ru1 115.58(15) . . ?
C12 N4 Ru1 126.17(18) . . ?
O11 N6 O3 120.3(2) . . ?
O11 N6 Ru1 119.21(17) . . ?
O3 N6 Ru1 120.46(16) . . ?
N4 C10 C13 123.4(2) . . ?
N4 C10 H10 118.3 . . ?
C13 C10 H10 118.3 . . ?
N4 C12 C14 119.0(3) . . ?
N4 C12 C16 120.5(2) . . ?
C14 C12 C16 120.5(3) . . ?
C10 C13 C18 118.3(3) . . ?
C10 C13 H13 120.9 . . ?
C18 C13 H13 120.9 . . ?
C18 C14 C12 121.9(3) . . ?
C18 C14 H14 119.1 . . ?
C12 C14 H14 119.1 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C18 C13 119.1(3) . . ?
C14 C18 H18 120.4 . . ?
C13 C18 H18 120.4 . . ?
Ru1 O1 Ru1 113.56(10) . 2_655 ?
N3 O2 Ru1 114.75(12) 2_655 . ?
O4 N3 O2 116.54(18) . 2_655 ?
O4 N3 Ru1 124.22(16) . . ?
O2 N3 Ru1 119.24(13) 2_655 . ?
O5 N5 Ru1 168.8(2) . . ?

_refine_diff_density_max         0.376
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.069

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kru090p
_database_code_depnum_ccdc_archive 'CCDC 1555057'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 N5 O6 Ru'
_chemical_formula_sum            'C12 H15 N5 O6 Ru'
_chemical_formula_weight         426.36

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.4624(3)
_cell_length_b                   9.9201(3)
_cell_length_c                   17.3772(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.2920(10)
_cell_angle_gamma                90
_cell_volume                     1626.59(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    9995
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.60

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.003
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_T_max  0.7283
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14043
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.274
_diffrn_reflns_theta_max         27.605
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3719
_reflns_number_gt                3564
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond 3.2k'
_computing_publication_material  'Diamond 3.2k'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0085P)²+1.3960P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3719
_refine_ls_number_parameters     224
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0470
_refine_ls_wR_factor_gt          0.0465
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.074
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.11929(2) 0.33304(2) 0.14248(2) 0.00800(5) Uani 1 1 d . . . . .
O1 O 0.04282(12) 0.31904(11) 0.03750(6) 0.0137(2) Uani 1 1 d D . . . .
H1 H -0.0389(14) 0.367(2) 0.0293(13) 0.036(6) Uiso 1 1 d D . . . .
N2A N 0.1931(12) 0.3695(10) 0.3091(11) 0.0112(3) Uani 0.285(14) 1 d . . P A 2
O31 O -0.17530(12) 0.41940(13) 0.12229(7) 0.0202(2) Uani 1 1 d . . . . .
O32 O -0.09770(12) 0.41337(12) 0.24174(6) 0.0181(2) Uani 1 1 d . . . . .
O41 O 0.20512(14) 0.57390(12) 0.06020(7) 0.0226(3) Uani 1 1 d . . . . .
O42 O 0.18798(15) 0.60922(12) 0.18081(7) 0.0252(3) Uani 1 1 d . . . . .
O2A O 0.186(2) 0.3539(19) 0.2469(7) 0.0112(3) Uani 0.285(14) 1 d . . P A 2
N3 N -0.07810(13) 0.39769(12) 0.17216(7) 0.0117(2) Uani 1 1 d . . . . .
N4 N 0.17783(13) 0.53255(13) 0.12416(7) 0.0128(2) Uani 1 1 d . . . . .
N5 N 0.31175(13) 0.26465(13) 0.10124(7) 0.0107(2) Uani 1 1 d . . . . .
N6 N 0.05061(13) 0.13162(13) 0.15892(7) 0.0103(2) Uani 1 1 d . . . . .
C51 C 0.34973(17) 0.30543(17) 0.03139(9) 0.0156(3) Uani 1 1 d . . . . .
H51 H 0.289391 0.365364 0.001642 0.019 Uiso 1 1 calc R U . . .
C52 C 0.47396(17) 0.26229(17) 0.00210(9) 0.0169(3) Uani 1 1 d . . . . .
H52 H 0.498128 0.293539 -0.046897 0.020 Uiso 1 1 calc R U . . .
C53 C 0.56391(16) 0.17322(15) 0.04406(9) 0.0131(3) Uani 1 1 d . . . . .
C54 C 0.52273(16) 0.13142(16) 0.11585(9) 0.0138(3) Uani 1 1 d . . . . .
H54 H 0.580431 0.070281 0.146287 0.017 Uiso 1 1 calc R U . . .
C55 C 0.39820(16) 0.17889(15) 0.14259(9) 0.0121(3) Uani 1 1 d . . . . .
H55 H 0.372525 0.150170 0.191802 0.015 Uiso 1 1 calc R U . . .
C56 C 0.69925(17) 0.12397(17) 0.01394(10) 0.0184(3) Uani 1 1 d . . . . .
H56A H 0.698523 0.143665 -0.041348 0.028 Uiso 1 1 calc R U . . .
H56B H 0.707711 0.026465 0.022113 0.028 Uiso 1 1 calc R U . . .
H56C H 0.779890 0.169612 0.041402 0.028 Uiso 1 1 calc R U . . .
C61 C 0.05437(16) 0.04028(15) 0.10201(8) 0.0116(3) Uani 1 1 d . . . . .
H61 H 0.099026 0.064031 0.056751 0.014 Uiso 1 1 calc R U . . .
C62 C -0.00426(16) -0.08715(15) 0.10670(9) 0.0138(3) Uani 1 1 d . . . . .
H62 H 0.001831 -0.149375 0.065527 0.017 Uiso 1 1 calc R U . . .
C63 C -0.07211(16) -0.12374(16) 0.17193(9) 0.0148(3) Uani 1 1 d . . . . .
C64 C -0.07127(17) -0.03028(16) 0.23207(9) 0.0153(3) Uani 1 1 d . . . . .
H64 H -0.113099 -0.052486 0.278454 0.018 Uiso 1 1 calc R U . . .
C65 C -0.00929(16) 0.09484(15) 0.22390(9) 0.0135(3) Uani 1 1 d . . . . .
H65 H -0.008873 0.157059 0.265474 0.016 Uiso 1 1 calc R U . . .
C66 C -0.14551(19) -0.25765(17) 0.17594(11) 0.0226(4) Uani 1 1 d . . . . .
H66A H -0.128074 -0.311019 0.130147 0.034 Uiso 1 1 calc R U . . .
H66B H -0.247641 -0.243275 0.177909 0.034 Uiso 1 1 calc R U . . .
H66C H -0.108669 -0.305963 0.222382 0.034 Uiso 1 1 calc R U . . .
O2B O 0.2150(3) 0.3840(3) 0.3034(3) 0.0112(3) Uani 0.715(14) 1 d . . P A 1
N2B N 0.1830(11) 0.3523(9) 0.2385(4) 0.0112(3) Uani 0.715(14) 1 d . . P A 1


_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 N2B 1.741(6) . ?
Ru1 O2A 1.888(10) . ?
Ru1 O1 1.9165(11) . ?
Ru1 N3 2.0761(12) . ?
Ru1 N4 2.0861(13) . ?
Ru1 N5 2.1179(12) . ?
Ru1 N6 2.1269(13) . ?
O1 H1 0.911(5) . ?
N2A O2A 1.089(17) . ?
O31 N3 1.2344(17) . ?
O32 N3 1.2468(16) . ?
O41 N4 1.2302(17) . ?
O42 N4 1.2419(17) . ?
N5 C55 1.3496(19) . ?
N5 C51 1.3532(19) . ?
N6 C61 1.3436(19) . ?
N6 C65 1.3510(19) . ?
C51 C52 1.383(2) . ?
C51 H51 0.9500 . ?
C52 C53 1.394(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.397(2) . ?
C53 C56 1.501(2) . ?
C54 C55 1.381(2) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C61 C62 1.385(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.392(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.397(2) . ?
C63 C66 1.503(2) . ?
C64 C65 1.385(2) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
O2B N2B 1.189(9) . ?

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
N2B Ru1 O1 177.2(2) . . ?
O2A Ru1 O1 176.7(4) . . ?
N2B Ru1 N3 88.9(3) . . ?
O2A Ru1 N3 88.3(6) . . ?
O1 Ru1 N3 88.64(5) . . ?
N2B Ru1 N4 88.0(4) . . ?
O2A Ru1 N4 88.2(7) . . ?
O1 Ru1 N4 90.53(5) . . ?
N3 Ru1 N4 89.94(5) . . ?
N2B Ru1 N5 96.6(3) . . ?
O2A Ru1 N5 97.2(6) . . ?
O1 Ru1 N5 85.85(5) . . ?
N3 Ru1 N5 174.48(5) . . ?
N4 Ru1 N5 90.42(5) . . ?
N2B Ru1 N6 93.5(4) . . ?
O2A Ru1 N6 93.3(7) . . ?
O1 Ru1 N6 87.85(5) . . ?
N3 Ru1 N6 88.12(5) . . ?
N4 Ru1 N6 177.50(5) . . ?
N5 Ru1 N6 91.36(5) . . ?
Ru1 O1 H1 111.5(15) . . ?
N2A O2A Ru1 164(2) . . ?
O31 N3 O32 120.12(13) . . ?
O31 N3 Ru1 121.09(10) . . ?
O32 N3 Ru1 118.78(10) . . ?
O41 N4 O42 120.19(13) . . ?
O41 N4 Ru1 122.02(10) . . ?
O42 N4 Ru1 117.76(10) . . ?
C55 N5 C51 118.36(13) . . ?
C55 N5 Ru1 121.60(10) . . ?
C51 N5 Ru1 120.04(10) . . ?
C61 N6 C65 117.96(13) . . ?
C61 N6 Ru1 120.63(10) . . ?
C65 N6 Ru1 121.16(10) . . ?
N5 C51 C52 121.84(14) . . ?
N5 C51 H51 119.1 . . ?
C52 C51 H51 119.1 . . ?
C51 C52 C53 120.39(14) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 H52 119.8 . . ?
C52 C53 C54 117.05(14) . . ?
C52 C53 C56 121.83(14) . . ?
C54 C53 C56 121.12(14) . . ?
C55 C54 C53 120.07(14) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
N5 C55 C54 122.28(14) . . ?
N5 C55 H55 118.9 . . ?
C54 C55 H55 118.9 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N6 C61 C62 122.64(14) . . ?
N6 C61 H61 118.7 . . ?
C62 C61 H61 118.7 . . ?
C61 C62 C63 119.80(14) . . ?
C61 C62 H62 120.1 . . ?
C63 C62 H62 120.1 . . ?
C62 C63 C64 117.32(14) . . ?
C62 C63 C66 120.74(15) . . ?
C64 C63 C66 121.92(15) . . ?
C65 C64 C63 119.80(14) . . ?
C65 C64 H64 120.1 . . ?
C63 C64 H64 120.1 . . ?
N6 C65 C64 122.36(14) . . ?
N6 C65 H65 118.8 . . ?
C64 C65 H65 118.8 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O2B N2B Ru1 169.7(5) . . ?

_refine_diff_density_max         0.470
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.064

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_art002b
_database_code_depnum_ccdc_archive 'CCDC 1546165'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 N5 O6 Ru'
_chemical_formula_sum            'C12 H15 N5 O6 Ru'
_chemical_formula_weight         426.36

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   28.1411(10)
_cell_length_b                   9.5372(3)
_cell_length_c                   13.4951(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.1040(10)
_cell_angle_gamma                90
_cell_volume                     3252.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9183
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.34

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.004
_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_T_max  0.8054
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12076
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.282
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             5873
_reflns_number_gt                5672
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.899
_reflns_Friedel_fraction_full    0.913

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond 3.2k'
_computing_publication_material  'Diamond 3.2k'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2528 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5873
_refine_ls_number_parameters     442
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.39637(2) 0.35561(4) 0.09818(2) 0.02137(12) Uani 1 1 d D . . . .
Ru2 Ru 0.62910(2) 0.63087(4) 0.01928(2) 0.02034(11) Uani 1 1 d . . . . .
O1 O 0.68825(15) 0.6351(4) 0.1634(3) 0.0324(9) Uani 1 1 d . . . . .
H1 H 0.715471 0.661337 0.157813 0.039 Uiso 1 1 calc R U . . .
N5 N 0.58009(18) 0.6300(4) -0.1173(4) 0.0284(11) Uani 1 1 d . . . . .
N6 N 0.68061(19) 0.5423(5) -0.0358(4) 0.0285(11) Uani 1 1 d . . . . .
N10 N 0.58161(18) 0.7218(4) 0.0895(4) 0.0263(10) Uani 1 1 d . . . . .
N18 N 0.61161(19) 0.4260(4) 0.0584(4) 0.0281(10) Uani 1 1 d . . . . .
N1 N 0.35986(17) 0.2222(4) -0.0411(3) 0.0223(9) Uani 1 1 d . . . . .
O10 O 0.55379(19) 0.6324(5) -0.2127(4) 0.0494(12) Uani 1 1 d . . . . .
N2 N 0.45157(18) 0.2009(5) 0.1770(4) 0.0277(10) Uani 1 1 d . . . . .
N3 N 0.44195(19) 0.4307(4) 0.0557(4) 0.0247(10) Uani 1 1 d . . . . .
O8 O 0.4789(2) 0.4744(5) 0.0493(4) 0.0494(12) Uani 1 1 d . . . . .
N12 N 0.42822(19) 0.4819(5) 0.2384(4) 0.0292(10) Uani 1 1 d . . . . .
O3 O 0.35289(16) 0.2730(4) 0.1586(4) 0.0320(9) Uani 1 1 d D . . . .
N4 N 0.33526(18) 0.5049(4) 0.0160(4) 0.0273(10) Uani 1 1 d . . . . .
C5 C 0.3773(2) 0.2136(5) -0.1196(4) 0.0239(11) Uani 1 1 d . . . . .
H5 H 0.407050 0.268429 -0.110849 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3167(2) 0.1475(6) -0.0547(5) 0.0297(13) Uani 1 1 d . . . . .
H6 H 0.303018 0.155905 -0.001988 0.036 Uiso 1 1 calc R U . . .
C14 C 0.2920(2) 0.0591(7) -0.1439(5) 0.0405(15) Uani 1 1 d . . . . .
H14 H 0.262583 0.004245 -0.150415 0.049 Uiso 1 1 calc R U . . .
C18 C 0.3539(2) 0.1286(5) -0.2125(5) 0.0289(12) Uani 1 1 d . . . . .
C20 C 0.3753(3) 0.1233(6) -0.2957(5) 0.0402(15) Uani 1 1 d . . . . .
H20A H 0.394071 0.034428 -0.288508 0.060 Uiso 1 1 calc R U . . .
H20B H 0.399879 0.201520 -0.283261 0.060 Uiso 1 1 calc R U . . .
H20C H 0.346122 0.130347 -0.369994 0.060 Uiso 1 1 calc R U . . .
C15 C 0.2628(3) 0.6441(6) 0.0078(7) 0.0486(19) Uani 1 1 d . . . . .
C16 C 0.3034(2) 0.5456(6) 0.0592(5) 0.0363(14) Uani 1 1 d . . . . .
H16 H 0.308198 0.506494 0.127695 0.044 Uiso 1 1 calc R U . . .
C1 C 0.3100(3) 0.0505(6) -0.2228(5) 0.0398(15) Uani 1 1 d . . . . .
H9 H 0.292560 -0.008879 -0.284901 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3282(3) 0.5575(7) -0.0808(6) 0.0447(16) Uani 1 1 d . . . . .
H2 H 0.350658 0.527009 -0.112395 0.054 Uiso 1 1 calc R U . . .
O5 O 0.45875(18) 0.1582(5) 0.2678(4) 0.0445(11) Uani 1 1 d . . . . .
O2 O 0.47736(18) 0.1526(4) 0.1302(4) 0.0439(11) Uani 1 1 d . . . . .
O4 O 0.4577(2) 0.5796(5) 0.2429(4) 0.0539(13) Uani 1 1 d . . . . .
O19 O 0.4177(3) 0.4640(6) 0.3145(5) 0.081(2) Uani 1 1 d . . . . .
C3 C 0.5912(4) 0.1588(8) 0.1079(9) 0.068(3) Uani 1 1 d . . . . .
H15 H 0.583289 0.069049 0.127294 0.081 Uiso 1 1 calc R U . . .
O6 O 0.72843(16) 0.5536(5) 0.0160(4) 0.0417(11) Uani 1 1 d . . . . .
C4 C 0.5201(2) 0.8430(5) 0.1834(5) 0.0305(13) Uani 1 1 d . . . . .
H4 H 0.499501 0.883811 0.215789 0.037 Uiso 1 1 calc R U . . .
O9 O 0.6625(2) 0.4727(6) -0.1204(4) 0.0599(14) Uani 1 1 d . . . . .
N11 N 0.6524(2) 0.8297(5) -0.0021(4) 0.0384(12) Uani 1 1 d . . . . .
O7 O 0.6190(2) 0.9111(5) -0.0647(5) 0.0618(14) Uani 1 1 d . . . . .
O12 O 0.6990(2) 0.8642(5) 0.0494(7) 0.082(2) Uani 1 1 d . . . . .
C9 C 0.4986(2) 0.8109(6) 0.0736(5) 0.0311(12) Uani 1 1 d . . . . .
C10 C 0.5741(3) 0.8130(7) 0.2461(5) 0.0417(15) Uani 1 1 d . . . . .
H10 H 0.590700 0.835422 0.322520 0.050 Uiso 1 1 calc R U . . .
C11 C 0.6031(2) 0.7522(6) 0.1990(5) 0.0352(13) Uani 1 1 d . . . . .
H11 H 0.639225 0.730430 0.243960 0.042 Uiso 1 1 calc R U . . .
C12 C 0.5682(3) 0.3567(6) -0.0110(6) 0.0443(17) Uani 1 1 d . . . . .
H12 H 0.544118 0.400259 -0.077609 0.053 Uiso 1 1 calc R U . . .
C13 C 0.6443(3) 0.3605(7) 0.1485(7) 0.0516(19) Uani 1 1 d . . . . .
H13 H 0.675300 0.407903 0.198361 0.062 Uiso 1 1 calc R U . . .
C17 C 0.5301(2) 0.7521(5) 0.0297(5) 0.0288(12) Uani 1 1 d . . . . .
H17 H 0.514476 0.731973 -0.047089 0.035 Uiso 1 1 calc R U . . .
C19 C 0.5579(4) 0.2195(7) 0.0140(7) 0.061(2) Uani 1 1 d . . . . .
H19 H 0.527345 0.170657 -0.035983 0.073 Uiso 1 1 calc R U . . .
C7 C 0.2570(3) 0.6973(8) -0.0906(7) 0.062(2) Uani 1 1 d . . . . .
H7 H 0.230084 0.764748 -0.127503 0.074 Uiso 1 1 calc R U . . .
C8 C 0.2890(3) 0.6559(8) -0.1375(7) 0.058(2) Uani 1 1 d . . . . .
H8 H 0.284643 0.692858 -0.206323 0.069 Uiso 1 1 calc R U . . .
C21 C 0.6351(3) 0.2236(9) 0.1737(8) 0.071(3) Uani 1 1 d . . . . .
C22 C 0.4399(3) 0.8385(8) 0.0001(7) 0.050(2) Uani 1 1 d . . . . .
H22A H 0.418632 0.766563 0.013639 0.075 Uiso 1 1 calc R U . . .
H22B H 0.433229 0.835598 -0.077540 0.075 Uiso 1 1 calc R U . . .
H22C H 0.430358 0.931143 0.017162 0.075 Uiso 1 1 calc R U . . .
C23 C 0.2288(3) 0.6864(8) 0.0625(8) 0.066(2) Uani 1 1 d . . . . .
H23A H 0.233368 0.786802 0.079734 0.099 Uiso 1 1 calc R U . . .
H23B H 0.239070 0.632780 0.130796 0.099 Uiso 1 1 calc R U . . .
H23C H 0.191588 0.667429 0.012682 0.099 Uiso 1 1 calc R U . . .
C24 C 0.6752(7) 0.1388(12) 0.2599(12) 0.123(5) Uani 1 1 d . . . . .
H24A H 0.658905 0.087525 0.300080 0.185 Uiso 1 1 calc R U . . .
H24B H 0.703215 0.199857 0.311144 0.185 Uiso 1 1 calc R U . . .
H24C H 0.690276 0.071949 0.226440 0.185 Uiso 1 1 calc R U . . .
H3 H 0.3619(13) 0.230(9) 0.217(4) 0.10(3) Uiso 1 1 d D . . . .


_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 N3 1.770(5) . ?
Ru1 O3 1.913(4) . ?
Ru1 N2 2.066(5) . ?
Ru1 N12 2.084(4) . ?
Ru1 N1 2.123(4) . ?
Ru1 N4 2.130(4) . ?
Ru2 N5 1.750(5) . ?
Ru2 O1 1.925(4) . ?
Ru2 N11 2.068(5) . ?
Ru2 N6 2.078(5) . ?
Ru2 N10 2.133(4) . ?
Ru2 N18 2.137(4) . ?
O1 H1 0.8400 . ?
N5 O10 1.169(6) . ?
N6 O6 1.218(6) . ?
N6 O9 1.221(6) . ?
N10 C17 1.344(7) . ?
N10 C11 1.359(7) . ?
N18 C13 1.314(8) . ?
N18 C12 1.342(9) . ?
N1 C6 1.349(7) . ?
N1 C5 1.351(7) . ?
N2 O5 1.220(6) . ?
N2 O2 1.242(6) . ?
N3 O8 1.158(6) . ?
N12 O19 1.199(7) . ?
N12 O4 1.231(7) . ?
O3 H3 0.821(14) . ?
N4 C16 1.325(7) . ?
N4 C2 1.330(8) . ?
C5 C18 1.392(7) . ?
C5 H5 0.9500 . ?
C6 C14 1.380(8) . ?
C6 H6 0.9500 . ?
C14 C1 1.368(9) . ?
C14 H14 0.9500 . ?
C18 C1 1.396(9) . ?
C18 C20 1.490(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C15 C7 1.363(11) . ?
C15 C16 1.404(9) . ?
C15 C23 1.500(11) . ?
C16 H16 0.9500 . ?
C1 H9 0.9500 . ?
C2 C8 1.392(9) . ?
C2 H2 0.9500 . ?
C3 C21 1.316(13) . ?
C3 C19 1.332(13) . ?
C3 H15 0.9500 . ?
C4 C9 1.366(8) . ?
C4 C10 1.406(9) . ?
C4 H4 0.9500 . ?
N11 O7 1.226(7) . ?
N11 O12 1.229(8) . ?
C9 C17 1.383(8) . ?
C9 C22 1.529(9) . ?
C10 C11 1.364(8) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C19 1.412(9) . ?
C12 H12 0.9500 . ?
C13 C21 1.402(10) . ?
C13 H13 0.9500 . ?
C17 H17 0.9500 . ?
C19 H19 0.9500 . ?
C7 C8 1.367(12) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C21 C24 1.457(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N3 Ru1 O3 174.2(2) . . ?
N3 Ru1 N2 88.18(19) . . ?
O3 Ru1 N2 87.89(18) . . ?
N3 Ru1 N12 88.7(2) . . ?
O3 Ru1 N12 87.21(19) . . ?
N2 Ru1 N12 91.12(18) . . ?
N3 Ru1 N1 95.34(18) . . ?
O3 Ru1 N1 88.81(17) . . ?
N2 Ru1 N1 89.38(17) . . ?
N12 Ru1 N1 175.97(18) . . ?
N3 Ru1 N4 95.44(19) . . ?
O3 Ru1 N4 88.63(17) . . ?
N2 Ru1 N4 175.97(18) . . ?
N12 Ru1 N4 90.73(17) . . ?
N1 Ru1 N4 88.52(17) . . ?
N5 Ru2 O1 174.0(2) . . ?
N5 Ru2 N11 90.5(2) . . ?
O1 Ru2 N11 86.3(2) . . ?
N5 Ru2 N6 88.4(2) . . ?
O1 Ru2 N6 86.60(18) . . ?
N11 Ru2 N6 90.49(19) . . ?
N5 Ru2 N10 96.46(19) . . ?
O1 Ru2 N10 88.57(17) . . ?
N11 Ru2 N10 89.34(19) . . ?
N6 Ru2 N10 175.17(18) . . ?
N5 Ru2 N18 95.5(2) . . ?
O1 Ru2 N18 87.72(18) . . ?
N11 Ru2 N18 174.0(2) . . ?
N6 Ru2 N18 89.41(17) . . ?
N10 Ru2 N18 90.25(16) . . ?
Ru2 O1 H1 109.5 . . ?
O10 N5 Ru2 169.5(4) . . ?
O6 N6 O9 119.1(5) . . ?
O6 N6 Ru2 121.8(4) . . ?
O9 N6 Ru2 119.1(4) . . ?
C17 N10 C11 117.0(5) . . ?
C17 N10 Ru2 122.8(4) . . ?
C11 N10 Ru2 120.3(4) . . ?
C13 N18 C12 117.6(5) . . ?
C13 N18 Ru2 121.3(4) . . ?
C12 N18 Ru2 121.0(4) . . ?
C6 N1 C5 118.4(5) . . ?
C6 N1 Ru1 119.6(4) . . ?
C5 N1 Ru1 122.0(3) . . ?
O5 N2 O2 120.8(5) . . ?
O5 N2 Ru1 120.7(4) . . ?
O2 N2 Ru1 118.6(4) . . ?
O8 N3 Ru1 166.4(4) . . ?
O19 N12 O4 118.7(5) . . ?
O19 N12 Ru1 121.8(4) . . ?
O4 N12 Ru1 119.6(4) . . ?
Ru1 O3 H3 129(2) . . ?
C16 N4 C2 119.0(5) . . ?
C16 N4 Ru1 120.9(4) . . ?
C2 N4 Ru1 120.1(4) . . ?
N1 C5 C18 123.5(5) . . ?
N1 C5 H5 118.3 . . ?
C18 C5 H5 118.3 . . ?
N1 C6 C14 121.3(6) . . ?
N1 C6 H6 119.4 . . ?
C14 C6 H6 119.4 . . ?
C1 C14 C6 119.9(6) . . ?
C1 C14 H14 120.1 . . ?
C6 C14 H14 120.1 . . ?
C5 C18 C1 116.5(5) . . ?
C5 C18 C20 120.8(5) . . ?
C1 C18 C20 122.7(5) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C15 C16 117.0(7) . . ?
C7 C15 C23 123.4(7) . . ?
C16 C15 C23 119.6(7) . . ?
N4 C16 C15 122.7(6) . . ?
N4 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C14 C1 C18 120.4(5) . . ?
C14 C1 H9 119.8 . . ?
C18 C1 H9 119.8 . . ?
N4 C2 C8 122.2(7) . . ?
N4 C2 H2 118.9 . . ?
C8 C2 H2 118.9 . . ?
C21 C3 C19 119.8(7) . . ?
C21 C3 H15 120.1 . . ?
C19 C3 H15 120.1 . . ?
C9 C4 C10 117.0(5) . . ?
C9 C4 H4 121.5 . . ?
C10 C4 H4 121.5 . . ?
O7 N11 O12 121.7(5) . . ?
O7 N11 Ru2 118.9(4) . . ?
O12 N11 Ru2 119.5(4) . . ?
C4 C9 C17 119.6(6) . . ?
C4 C9 C22 120.1(6) . . ?
C17 C9 C22 120.3(6) . . ?
C11 C10 C4 121.0(6) . . ?
C11 C10 H10 119.5 . . ?
C4 C10 H10 119.5 . . ?
N10 C11 C10 121.8(6) . . ?
N10 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
N18 C12 C19 120.5(7) . . ?
N18 C12 H12 119.7 . . ?
C19 C12 H12 119.7 . . ?
N18 C13 C21 122.6(8) . . ?
N18 C13 H13 118.7 . . ?
C21 C13 H13 118.7 . . ?
N10 C17 C9 123.7(5) . . ?
N10 C17 H17 118.2 . . ?
C9 C17 H17 118.2 . . ?
C3 C19 C12 119.9(8) . . ?
C3 C19 H19 120.0 . . ?
C12 C19 H19 120.0 . . ?
C15 C7 C8 121.4(6) . . ?
C15 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C2 117.7(7) . . ?
C7 C8 H8 121.1 . . ?
C2 C8 H8 121.1 . . ?
C3 C21 C13 119.4(7) . . ?
C3 C21 C24 116.4(8) . . ?
C13 C21 C24 123.4(9) . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C15 C23 H23A 109.5 . . ?
C15 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C15 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         1.014
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.067

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_testdo
_database_code_depnum_ccdc_archive 'CCDC 1546168'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 N5 O6 Ru'
_chemical_formula_sum            'C12 H15 N5 O6 Ru'
_chemical_formula_weight         426.36

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.4590(2)
_cell_length_b                   9.9164(3)
_cell_length_c                   17.3619(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.2700(10)
_cell_angle_gamma                90
_cell_volume                     1624.01(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    9824
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.57

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.005
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11587
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.276
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3069
_reflns_number_gt                2936
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond 3.2k'
_computing_publication_material  'Diamond 3.2k'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0130P)²+1.3950P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3069
_refine_ls_number_parameters     223
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0462
_refine_ls_wR_factor_gt          0.0457
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.11988(2) 0.33246(2) 0.14294(2) 0.00752(6) Uani 1 1 d . . . . .
O1 O 0.04294(13) 0.31820(12) 0.03786(7) 0.0134(3) Uani 1 1 d D . . . .
H1 H -0.0394(15) 0.366(2) 0.0291(14) 0.037(7) Uiso 1 1 d D . . . .
O2 O 0.21110(13) 0.38193(12) 0.30412(7) 0.0159(3) Uani 1 1 d . . . . .
O31 O -0.17482(13) 0.41841(13) 0.12255(7) 0.0199(3) Uani 1 1 d . . . . .
O32 O -0.09773(13) 0.41306(13) 0.24209(7) 0.0177(3) Uani 1 1 d . . . . .
O41 O 0.20529(15) 0.57248(13) 0.05976(7) 0.0226(3) Uani 1 1 d . . . . .
O42 O 0.18713(16) 0.60999(13) 0.18012(8) 0.0239(3) Uani 1 1 d . . . . .
N2 N 0.18422(15) 0.35363(13) 0.24040(8) 0.0099(3) Uani 1 1 d . . . . .
N3 N -0.07782(15) 0.39711(14) 0.17242(8) 0.0118(3) Uani 1 1 d . . . . .
N4 N 0.17772(15) 0.53196(14) 0.12381(8) 0.0131(3) Uani 1 1 d . . . . .
N5 N 0.31183(14) 0.26391(14) 0.10113(8) 0.0106(3) Uani 1 1 d . . . . .
N6 N 0.05089(14) 0.13098(14) 0.15941(8) 0.0098(3) Uani 1 1 d . . . . .
C51 C 0.34942(19) 0.30430(18) 0.03112(10) 0.0150(4) Uani 1 1 d . . . . .
H51 H 0.288765 0.363987 0.001352 0.018 Uiso 1 1 calc R U . . .
C52 C 0.47353(19) 0.26133(18) 0.00157(10) 0.0163(4) Uani 1 1 d . . . . .
H52 H 0.497200 0.292426 -0.047600 0.020 Uiso 1 1 calc R U . . .
C53 C 0.56394(19) 0.17284(16) 0.04339(10) 0.0129(3) Uani 1 1 d . . . . .
C54 C 0.52323(18) 0.13129(17) 0.11528(10) 0.0134(3) Uani 1 1 d . . . . .
H54 H 0.581250 0.070286 0.145680 0.016 Uiso 1 1 calc R U . . .
C55 C 0.39902(19) 0.17851(16) 0.14233(10) 0.0121(3) Uani 1 1 d . . . . .
H55 H 0.373956 0.149893 0.191731 0.015 Uiso 1 1 calc R U . . .
C56 C 0.69904(19) 0.12390(19) 0.01304(11) 0.0181(4) Uani 1 1 d . . . . .
H56A H 0.697605 0.142875 -0.042412 0.027 Uiso 1 1 calc R U . . .
H56B H 0.708163 0.026509 0.021623 0.027 Uiso 1 1 calc R U . . .
H56C H 0.779689 0.170301 0.040050 0.027 Uiso 1 1 calc R U . . .
C61 C 0.05369(17) 0.03996(17) 0.10226(9) 0.0114(3) Uani 1 1 d . . . . .
H61 H 0.097745 0.063891 0.056779 0.014 Uiso 1 1 calc R U . . .
C62 C -0.00496(18) -0.08704(17) 0.10699(10) 0.0132(3) Uani 1 1 d . . . . .
H62 H 0.000561 -0.149083 0.065626 0.016 Uiso 1 1 calc R U . . .
C63 C -0.07207(18) -0.12398(18) 0.17237(10) 0.0145(4) Uani 1 1 d . . . . .
C64 C -0.07052(18) -0.03093(18) 0.23275(10) 0.0154(4) Uani 1 1 d . . . . .
H64 H -0.111999 -0.053303 0.279262 0.018 Uiso 1 1 calc R U . . .
C65 C -0.00854(18) 0.09360(17) 0.22459(10) 0.0131(3) Uani 1 1 d . . . . .
H65 H -0.007541 0.155536 0.266373 0.016 Uiso 1 1 calc R U . . .
C66 C -0.1461(2) -0.25784(18) 0.17653(12) 0.0223(4) Uani 1 1 d . . . . .
H66A H -0.126519 -0.312515 0.131526 0.033 Uiso 1 1 calc R U . . .
H66B H -0.248525 -0.243187 0.176919 0.033 Uiso 1 1 calc R U . . .
H66C H -0.111534 -0.304970 0.223847 0.033 Uiso 1 1 calc R U . . .


_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 N2 1.7676(14) . ?
Ru1 O1 1.9184(12) . ?
Ru1 N3 2.0767(14) . ?
Ru1 N4 2.0858(14) . ?
Ru1 N5 2.1170(14) . ?
Ru1 N6 2.1276(14) . ?
O1 H1 0.913(5) . ?
O2 N2 1.1512(19) . ?
O31 N3 1.2320(19) . ?
O32 N3 1.2480(18) . ?
O41 N4 1.2285(19) . ?
O42 N4 1.2447(19) . ?
N5 C55 1.350(2) . ?
N5 C51 1.352(2) . ?
N6 C61 1.343(2) . ?
N6 C65 1.352(2) . ?
C51 C52 1.383(2) . ?
C51 H51 0.9500 . ?
C52 C53 1.391(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.396(2) . ?
C53 C56 1.499(2) . ?
C54 C55 1.379(2) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C61 C62 1.381(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.390(3) . ?
C62 H62 0.9500 . ?
C63 C64 1.396(2) . ?
C63 C66 1.505(2) . ?
C64 C65 1.379(2) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?

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
N2 Ru1 O1 176.69(5) . . ?
N2 Ru1 N3 88.83(6) . . ?
O1 Ru1 N3 88.41(5) . . ?
N2 Ru1 N4 87.94(6) . . ?
O1 Ru1 N4 90.22(5) . . ?
N3 Ru1 N4 89.89(5) . . ?
N2 Ru1 N5 97.09(6) . . ?
O1 Ru1 N5 85.67(5) . . ?
N3 Ru1 N5 174.08(5) . . ?
N4 Ru1 N5 90.46(5) . . ?
N2 Ru1 N6 94.02(6) . . ?
O1 Ru1 N6 87.72(5) . . ?
N3 Ru1 N6 88.05(5) . . ?
N4 Ru1 N6 177.13(5) . . ?
N5 Ru1 N6 91.38(5) . . ?
Ru1 O1 H1 112.3(16) . . ?
O2 N2 Ru1 169.91(13) . . ?
O31 N3 O32 120.08(14) . . ?
O31 N3 Ru1 121.12(11) . . ?
O32 N3 Ru1 118.79(11) . . ?
O41 N4 O42 120.01(14) . . ?
O41 N4 Ru1 122.02(11) . . ?
O42 N4 Ru1 117.95(11) . . ?
C55 N5 C51 118.11(14) . . ?
C55 N5 Ru1 121.70(11) . . ?
C51 N5 Ru1 120.18(11) . . ?
C61 N6 C65 117.79(14) . . ?
C61 N6 Ru1 120.58(11) . . ?
C65 N6 Ru1 121.37(11) . . ?
N5 C51 C52 121.97(16) . . ?
N5 C51 H51 119.0 . . ?
C52 C51 H51 119.0 . . ?
C51 C52 C53 120.43(16) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 H52 119.8 . . ?
C52 C53 C54 116.94(16) . . ?
C52 C53 C56 121.86(16) . . ?
C54 C53 C56 121.20(16) . . ?
C55 C54 C53 120.20(16) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
N5 C55 C54 122.34(16) . . ?
N5 C55 H55 118.8 . . ?
C54 C55 H55 118.8 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N6 C61 C62 122.61(15) . . ?
N6 C61 H61 118.7 . . ?
C62 C61 H61 118.7 . . ?
C61 C62 C63 119.91(15) . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C62 C63 C64 117.33(16) . . ?
C62 C63 C66 120.93(16) . . ?
C64 C63 C66 121.73(16) . . ?
C65 C64 C63 119.72(16) . . ?
C65 C64 H64 120.1 . . ?
C63 C64 H64 120.1 . . ?
N6 C65 C64 122.54(15) . . ?
N6 C65 H65 118.7 . . ?
C64 C65 H65 118.7 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_refine_diff_density_max         0.346
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.062

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bor165
_database_code_depnum_ccdc_archive 'CCDC 1546166'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H17 Cl2 N5 O6 Ru'
_chemical_formula_sum            'C13 H17 Cl2 N5 O6 Ru'
_chemical_formula_weight         511.29

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   9.7379(10)
_cell_length_b                   10.3204(12)
_cell_length_c                   20.607(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.386(3)
_cell_angle_gamma                90
_cell_volume                     2070.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      27.56

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.052
_shelx_estimated_absorpt_T_min   0.893
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4921
_exptl_absorpt_correction_T_max  0.6978
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12999
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.977
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3917
_reflns_number_gt                3452
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond 3.2k'
_computing_publication_material  'Diamond 3.2k'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0713P)²+4.3230P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3917
_refine_ls_number_parameters     275
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.001
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.87465(4) 0.61288(4) 0.33946(2) 0.03817(17) Uani 1 1 d . . . . .
O2 O 0.8180(4) 0.6263(4) 0.42835(18) 0.0526(9) Uani 1 1 d . . . . .
H2 H 0.734868 0.605466 0.431293 0.063 Uiso 1 1 calc DR U . . .
N1 N 0.9240(4) 0.5951(4) 0.2578(2) 0.0427(9) Uani 1 1 d . . . . .
N2 N 1.0706(4) 0.6763(4) 0.37165(19) 0.0427(9) Uani 1 1 d . . . . .
O4 O 0.9483(5) 0.5714(5) 0.20478(19) 0.0684(11) Uani 1 1 d . . . . .
N5 N 0.9286(5) 0.4209(4) 0.3566(2) 0.0509(10) Uani 1 1 d . . . . .
N6 N 0.8084(4) 0.8077(4) 0.3279(2) 0.0431(9) Uani 1 1 d . . . . .
O7 O 0.9055(7) 0.3695(5) 0.4085(3) 0.0943(19) Uani 1 1 d . . . . .
O8 O 0.9785(6) 0.3570(4) 0.3132(2) 0.0771(14) Uani 1 1 d . . . . .
C11 C 0.8254(6) 0.8928(5) 0.3766(3) 0.0548(13) Uani 1 1 d . . . . .
H11 H 0.876538 0.867261 0.413837 0.066 Uiso 1 1 calc R U . . .
C12 C 1.1189(6) 0.6411(6) 0.4305(3) 0.0588(14) Uani 1 1 d . . . . .
H12 H 1.064281 0.587411 0.457418 0.071 Uiso 1 1 calc R U . . .
N13 N 0.6787(5) 0.5481(5) 0.3166(3) 0.0576(12) Uani 1 1 d . . . . .
C15 C 0.7385(6) 0.8480(6) 0.2752(3) 0.0544(13) Uani 1 1 d . . . . .
H15 H 0.728101 0.789759 0.239856 0.065 Uiso 1 1 calc R U . . .
C16 C 1.2784(6) 0.7934(7) 0.3556(3) 0.0629(15) Uani 1 1 d . . . . .
H16 H 1.330963 0.848939 0.328630 0.076 Uiso 1 1 calc R U . . .
O17 O 0.5982(6) 0.5207(7) 0.3599(3) 0.107(2) Uani 1 1 d . . . . .
C18 C 0.7710(7) 1.0165(6) 0.3742(3) 0.0617(15) Uani 1 1 d . . . . .
H18 H 0.785102 1.074472 0.409448 0.074 Uiso 1 1 calc R U . . .
O19 O 0.6448(5) 0.5319(7) 0.2604(3) 0.0977(18) Uani 1 1 d . . . . .
C20 C 1.1497(6) 0.7520(6) 0.3355(3) 0.0530(13) Uani 1 1 d . . . . .
H20 H 1.116666 0.778705 0.294147 0.064 Uiso 1 1 calc R U . . .
C3 C 1.3309(5) 0.7531(6) 0.4159(3) 0.0509(13) Uani 1 1 d . . . . .
C4 C 1.2461(7) 0.6815(7) 0.4524(3) 0.0676(17) Uani 1 1 d . . . . .
H4 H 1.274673 0.657655 0.494918 0.081 Uiso 1 1 calc R U . . .
C5 C 0.6960(6) 1.0554(5) 0.3206(3) 0.0593(14) Uani 1 1 d . . . . .
C6 C 0.6818(6) 0.9679(6) 0.2701(3) 0.0625(15) Uani 1 1 d . . . . .
H6 H 0.632628 0.991670 0.231931 0.075 Uiso 1 1 calc R U . . .
C7 C 1.4691(8) 0.8027(9) 0.4383(5) 0.095(3) Uani 1 1 d . . . . .
H7A H 1.476697 0.794085 0.485500 0.142 Uiso 1 1 calc R U . . .
H7B H 1.478391 0.894145 0.426183 0.142 Uiso 1 1 calc R U . . .
H7C H 1.541908 0.752215 0.417577 0.142 Uiso 1 1 calc R U . . .
C8 C 0.6307(9) 1.1883(7) 0.3179(5) 0.090(2) Uani 1 1 d . . . . .
H8A H 0.605232 1.208728 0.273001 0.134 Uiso 1 1 calc R U . . .
H8B H 0.696263 1.252961 0.334036 0.134 Uiso 1 1 calc R U . . .
H8C H 0.548445 1.189177 0.345036 0.134 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6655(6) 0.6558(6) 0.5940(2) 0.1155(19) Uani 0.642(12) 1 d D . P A 2
Cl2 Cl 0.7479(10) 0.9176(6) 0.5612(3) 0.147(4) Uani 0.642(12) 1 d D . P A 2
C2 C 0.7967(15) 0.7589(13) 0.5688(6) 0.089(5) Uani 0.642(12) 1 d D . P A 2
H2A H 0.873461 0.753575 0.600454 0.107 Uiso 0.642(12) 1 calc R U P A 2
H2B H 0.831299 0.728100 0.526458 0.107 Uiso 0.642(12) 1 calc R U P A 2
Cl3 Cl 0.884(2) 0.9612(11) 0.5398(5) 0.167(7) Uani 0.358(12) 1 d D . P A 1
Cl4 Cl 0.6780(13) 0.795(3) 0.5987(6) 0.244(16) Uani 0.358(12) 1 d D . P A 1
C1 C 0.823(3) 0.805(3) 0.5517(15) 0.17(2) Uani 0.358(12) 1 d D . P A 1
H1A H 0.802950 0.766157 0.508766 0.206 Uiso 0.358(12) 1 calc DR U P A 1
H1B H 0.896704 0.753020 0.572323 0.206 Uiso 0.358(12) 1 calc R U P A 1


_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 N1 1.762(4) . ?
Ru1 O2 1.922(4) . ?
Ru1 N13 2.073(5) . ?
Ru1 N5 2.079(5) . ?
Ru1 N2 2.119(4) . ?
Ru1 N6 2.125(4) . ?
O2 H2 0.8400 . ?
N1 O4 1.146(6) . ?
N2 C20 1.329(7) . ?
N2 C12 1.347(7) . ?
N5 O7 1.215(7) . ?
N5 O8 1.216(6) . ?
N6 C11 1.342(7) . ?
N6 C15 1.343(7) . ?
C11 C18 1.382(8) . ?
C11 H11 0.9500 . ?
C12 C4 1.380(9) . ?
C12 H12 0.9500 . ?
N13 O19 1.214(7) . ?
N13 O17 1.224(7) . ?
C15 C6 1.359(8) . ?
C15 H15 0.9500 . ?
C16 C20 1.384(8) . ?
C16 C3 1.405(8) . ?
C16 H16 0.9500 . ?
C18 C5 1.381(9) . ?
C18 H18 0.9500 . ?
C20 H20 0.9500 . ?
C3 C4 1.342(9) . ?
C3 C7 1.508(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(9) . ?
C5 C8 1.512(9) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cl1 C2 1.745(15) . ?
Cl2 C2 1.712(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
Cl3 C1 1.734(18) . ?
Cl4 C1 1.722(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
N1 Ru1 O2 177.99(17) . . ?
N1 Ru1 N13 90.3(2) . . ?
O2 Ru1 N13 88.3(2) . . ?
N1 Ru1 N5 89.62(19) . . ?
O2 Ru1 N5 88.87(18) . . ?
N13 Ru1 N5 87.85(19) . . ?
N1 Ru1 N2 94.61(17) . . ?
O2 Ru1 N2 86.74(16) . . ?
N13 Ru1 N2 174.87(19) . . ?
N5 Ru1 N2 90.88(17) . . ?
N1 Ru1 N6 94.36(17) . . ?
O2 Ru1 N6 87.11(16) . . ?
N13 Ru1 N6 90.08(17) . . ?
N5 Ru1 N6 175.53(17) . . ?
N2 Ru1 N6 90.84(15) . . ?
Ru1 O2 H2 109.5 . . ?
O4 N1 Ru1 172.7(4) . . ?
C20 N2 C12 117.5(5) . . ?
C20 N2 Ru1 122.0(3) . . ?
C12 N2 Ru1 120.4(4) . . ?
O7 N5 O8 119.2(5) . . ?
O7 N5 Ru1 121.2(4) . . ?
O8 N5 Ru1 119.6(4) . . ?
C11 N6 C15 117.4(5) . . ?
C11 N6 Ru1 120.0(4) . . ?
C15 N6 Ru1 122.4(4) . . ?
N6 C11 C18 122.2(6) . . ?
N6 C11 H11 118.9 . . ?
C18 C11 H11 118.9 . . ?
N2 C12 C4 121.4(6) . . ?
N2 C12 H12 119.3 . . ?
C4 C12 H12 119.3 . . ?
O19 N13 O17 119.4(6) . . ?
O19 N13 Ru1 120.3(4) . . ?
O17 N13 Ru1 120.1(5) . . ?
N6 C15 C6 123.3(5) . . ?
N6 C15 H15 118.4 . . ?
C6 C15 H15 118.4 . . ?
C20 C16 C3 119.8(6) . . ?
C20 C16 H16 120.1 . . ?
C3 C16 H16 120.1 . . ?
C5 C18 C11 119.8(6) . . ?
C5 C18 H18 120.1 . . ?
C11 C18 H18 120.1 . . ?
N2 C20 C16 122.8(5) . . ?
N2 C20 H20 118.6 . . ?
C16 C20 H20 118.6 . . ?
C4 C3 C16 115.9(5) . . ?
C4 C3 C7 124.6(6) . . ?
C16 C3 C7 119.2(6) . . ?
C3 C4 C12 122.5(6) . . ?
C3 C4 H4 118.7 . . ?
C12 C4 H4 118.7 . . ?
C18 C5 C6 117.5(5) . . ?
C18 C5 C8 120.8(6) . . ?
C6 C5 C8 121.6(6) . . ?
C15 C6 C5 119.8(6) . . ?
C15 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Cl2 C2 Cl1 114.0(8) . . ?
Cl2 C2 H2A 108.7 . . ?
Cl1 C2 H2A 108.7 . . ?
Cl2 C2 H2B 108.7 . . ?
Cl1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
Cl4 C1 Cl3 115(2) . . ?
Cl4 C1 H1A 108.6 . . ?
Cl3 C1 H1A 108.6 . . ?
Cl4 C1 H1B 108.6 . . ?
Cl3 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?

_refine_diff_density_max         0.943
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.155

