# 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 2020

####################################################################### 
# 
# 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_bra008_150k_ma1
_database_code_depnum_ccdc_archive 'CCDC 2016494'
loop_
_audit_author_name
_audit_author_address
'Vladislav Komarov'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2020-02-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Pt, F H12 N5 O Ru'
_chemical_formula_sum            'Cl6 H12 F N5 O Pt Ru'
_chemical_formula_weight         626.01
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pt Pt -1.7033 8.3905 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.0583(5)
_cell_length_b                   8.7624(6)
_cell_length_c                   22.0421(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1363.25(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   0.705
_shelx_estimated_absorpt_T_min   0.474
_exptl_absorpt_coefficient_mu    12.528
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0830 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.7589.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 -1.00 0.00 0.0130
1.00 1.00 2.00 0.0250
1.00 1.00 0.00 0.0150
-1.00 -1.00 0.00 0.0250
0.00 0.00 -1.00 0.0300
0.00 0.00 1.00 0.0520
-2.00 2.00 -1.00 0.0160

_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.650
_diffrn_reflns_theta_min         1.848
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                3651
_reflns_number_total             4053
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details 
;
 Flack x determined using 1407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(3)
_refine_ls_extinction_coef       0.00028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0020P)²+4.4430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0359
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2.a Idealised Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C), N2(H2A,H2B,H2C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pt1 Pt 0.65885(3) 0.85710(2) 0.87653(2) 0.00740(5) Uani 1 1 d . . . . .
Ru1 Ru 1.13558(6) 0.36598(5) 0.87831(2) 0.00773(9) Uani 1 1 d . . . . .
Cl5 Cl 0.4228(2) 0.79590(19) 0.80721(7) 0.0139(3) Uani 1 1 d . . . . .
Cl6 Cl 0.8922(2) 0.91791(18) 0.94609(7) 0.0131(3) Uani 1 1 d . . . . .
Cl3 Cl 0.6515(2) 0.60997(14) 0.91437(6) 0.0121(3) Uani 1 1 d . . . . .
Cl2 Cl 0.4253(2) 0.92232(19) 0.94550(7) 0.0139(3) Uani 1 1 d . . . . .
Cl1 Cl 0.6650(2) 1.10473(15) 0.83807(7) 0.0162(3) Uani 1 1 d . . . . .
Cl4 Cl 0.8926(2) 0.79128(19) 0.80675(7) 0.0141(3) Uani 1 1 d . . . . .
F1 F 1.3281(6) 0.3135(4) 0.93599(15) 0.0160(8) Uani 1 1 d . . . . .
O1 O 0.8374(7) 0.4342(5) 0.79332(18) 0.0175(9) Uani 1 1 d . . . . .
N1 N 1.1512(8) 0.5856(5) 0.9160(2) 0.0104(10) Uani 1 1 d . . . . .
H1A H 1.1707 0.6551 0.8860 0.012 Uiso 1 1 calc R U . . .
H1B H 1.2489 0.5896 0.9429 0.012 Uiso 1 1 calc R U . . .
H1C H 1.0408 0.6072 0.9355 0.012 Uiso 1 1 calc R U . . .
N3 N 1.1576(8) 0.1381(5) 0.8488(2) 0.0133(9) Uani 1 1 d . . . . .
H3A H 1.2023 0.1361 0.8101 0.016 Uiso 1 1 calc R U . . .
H3B H 1.0414 0.0933 0.8501 0.016 Uiso 1 1 calc R U . . .
H3C H 1.2387 0.0865 0.8735 0.016 Uiso 1 1 calc R U . . .
N2 N 1.3609(8) 0.4191(6) 0.8200(2) 0.0128(11) Uani 1 1 d . . . . .
H2A H 1.3382 0.3785 0.7827 0.015 Uiso 1 1 calc R U . . .
H2B H 1.4703 0.3797 0.8353 0.015 Uiso 1 1 calc R U . . .
H2C H 1.3719 0.5223 0.8168 0.015 Uiso 1 1 calc R U . . .
N5 N 0.9589(7) 0.4099(6) 0.8269(2) 0.0100(11) Uani 1 1 d . . . . .
N4 N 0.9414(8) 0.3031(6) 0.9464(2) 0.0151(12) Uani 1 1 d . . . . .
H4A H 0.9005 0.2061 0.9396 0.018 Uiso 1 1 calc R U . . .
H4B H 0.8408 0.3680 0.9458 0.018 Uiso 1 1 calc R U . . .
H4C H 0.9991 0.3080 0.9833 0.018 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
Pt1 Cl5 2.3231(16) . ?
Pt1 Cl6 2.3126(15) . ?
Pt1 Cl3 2.3210(13) . ?
Pt1 Cl2 2.3140(16) . ?
Pt1 Cl1 2.3300(14) . ?
Pt1 Cl4 2.3281(15) . ?
Ru1 F1 1.917(4) . ?
Ru1 N1 2.099(5) . ?
Ru1 N3 2.105(5) . ?
Ru1 N2 2.097(5) . ?
Ru1 N5 1.728(5) . ?
Ru1 N4 2.107(5) . ?
O1 N5 1.153(7) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?

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
Cl5 Pt1 Cl1 89.37(6) . . ?
Cl5 Pt1 Cl4 90.94(5) . . ?
Cl6 Pt1 Cl5 179.60(6) . . ?
Cl6 Pt1 Cl3 89.58(6) . . ?
Cl6 Pt1 Cl2 90.86(5) . . ?
Cl6 Pt1 Cl1 90.77(6) . . ?
Cl6 Pt1 Cl4 89.44(6) . . ?
Cl3 Pt1 Cl5 90.28(6) . . ?
Cl3 Pt1 Cl1 179.65(6) . . ?
Cl3 Pt1 Cl4 91.27(6) . . ?
Cl2 Pt1 Cl5 88.76(6) . . ?
Cl2 Pt1 Cl3 88.77(6) . . ?
Cl2 Pt1 Cl1 91.27(6) . . ?
Cl2 Pt1 Cl4 179.70(6) . . ?
Cl4 Pt1 Cl1 88.69(6) . . ?
F1 Ru1 N1 85.39(18) . . ?
F1 Ru1 N3 85.70(17) . . ?
F1 Ru1 N2 85.5(2) . . ?
F1 Ru1 N4 85.73(18) . . ?
N1 Ru1 N3 171.0(2) . . ?
N1 Ru1 N4 89.5(2) . . ?
N3 Ru1 N4 91.1(2) . . ?
N2 Ru1 N1 90.0(2) . . ?
N2 Ru1 N3 88.0(2) . . ?
N2 Ru1 N4 171.3(2) . . ?
N5 Ru1 F1 178.7(2) . . ?
N5 Ru1 N1 95.4(2) . . ?
N5 Ru1 N3 93.5(2) . . ?
N5 Ru1 N2 95.5(2) . . ?
N5 Ru1 N4 93.2(2) . . ?
Ru1 N1 H1A 109.5 . . ?
Ru1 N1 H1B 109.5 . . ?
Ru1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Ru1 N3 H3A 109.5 . . ?
Ru1 N3 H3B 109.5 . . ?
Ru1 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Ru1 N2 H2A 109.5 . . ?
Ru1 N2 H2B 109.5 . . ?
Ru1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
O1 N5 Ru1 177.4(5) . . ?
Ru1 N4 H4A 109.5 . . ?
Ru1 N4 H4B 109.5 . . ?
Ru1 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_aptcl4
_database_code_depnum_ccdc_archive 'CCDC 2016496'
loop_
_audit_author_name
_audit_author_address
'Vladislav Komarov'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2020-02-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Pt, F H12 N5 O Ru'
_chemical_formula_sum            'Cl4 H12 F N5 O Pt Ru'
_chemical_formula_weight         555.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pt Pt -1.7033 8.3905 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.1354(13)
_cell_length_b                   17.5637(18)
_cell_length_c                   8.1749(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1168.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    905
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      3.40
_shelx_estimated_absorpt_T_max   0.676
_shelx_estimated_absorpt_T_min   0.305
_exptl_absorpt_coefficient_mu    14.157
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1189 before and 0.0768 after correction. The Ratio of minimum to maximum transmission is 0.5715. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.157
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2669
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.345
_diffrn_reflns_theta_min         2.319
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                1025
_reflns_number_total             1253
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.233
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 
;
 Flack x determined using 420 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1253
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      0.831
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0685
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pt1 Pt 1.000000 0.62394(5) 0.29281(4) 0.0097(2) Uani 1 2 d S T P . .
Ru1 Ru 0.500000 0.37984(11) 0.32922(18) 0.0085(6) Uani 1 2 d S T P . .
Cl2 Cl 0.7173(3) 0.6290(2) 0.2975(7) 0.0154(7) Uani 1 1 d . . . . .
Cl1 Cl 1.000000 0.5706(4) 0.5511(7) 0.0142(13) Uani 1 2 d S T P . .
Cl3 Cl 1.000000 0.6714(4) 0.0255(7) 0.0146(12) Uani 1 2 d S T P . .
F1 F 0.500000 0.4538(7) 0.1493(14) 0.010(3) Uani 1 2 d S T P . .
N3 N 0.6858(14) 0.3228(9) 0.1973(16) 0.020(4) Uani 1 1 d . . . . .
H3A H 0.748005 0.298369 0.264183 0.025 Uiso 1 1 calc GR . . . .
H3B H 0.743542 0.355480 0.144015 0.025 Uiso 1 1 calc GR . . . .
H3C H 0.641529 0.291311 0.129802 0.025 Uiso 1 1 calc GR . . . .
N5 N 0.500000 0.3115(11) 0.483(2) 0.007(4) Uani 1 2 d S TU P . .
N1 N 0.6810(14) 0.4497(8) 0.4295(16) 0.018(3) Uani 1 1 d . . . . .
H1A H 0.694796 0.488872 0.367944 0.022 Uiso 1 1 calc GR . . . .
H1B H 0.771793 0.424774 0.436350 0.022 Uiso 1 1 calc GR . . . .
H1C H 0.651148 0.464161 0.525457 0.022 Uiso 1 1 calc GR . . . .
O1 O 0.500000 0.2625(9) 0.5754(18) 0.019(4) Uani 1 2 d S T P . .


_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
Pt1 Cl2 2.302(3) . ?
Pt1 Cl2 2.302(3) 3_755 ?
Pt1 Cl1 2.310(6) . ?
Pt1 Cl3 2.339(6) . ?
Ru1 F1 1.963(12) . ?
Ru1 N3 2.110(12) 3_655 ?
Ru1 N3 2.110(12) . ?
Ru1 N5 1.738(19) . ?
Ru1 N1 2.084(13) . ?
Ru1 N1 2.084(13) 3_655 ?
N5 O1 1.15(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
Cl2 Pt1 Cl2 175.2(2) . 3_755 ?
Cl2 Pt1 Cl1 90.02(14) 3_755 . ?
Cl2 Pt1 Cl1 90.02(14) . . ?
Cl2 Pt1 Cl3 90.11(14) . . ?
Cl2 Pt1 Cl3 90.11(14) 3_755 . ?
Cl1 Pt1 Cl3 177.0(2) . . ?
F1 Ru1 N3 86.1(5) . . ?
F1 Ru1 N3 86.1(5) . 3_655 ?
F1 Ru1 N1 84.6(5) . . ?
F1 Ru1 N1 84.6(5) . 3_655 ?
N3 Ru1 N3 91.5(7) . 3_655 ?
N5 Ru1 F1 177.8(7) . . ?
N5 Ru1 N3 92.4(6) . . ?
N5 Ru1 N3 92.4(6) . 3_655 ?
N5 Ru1 N1 97.0(6) . . ?
N5 Ru1 N1 97.0(6) . 3_655 ?
N1 Ru1 N3 88.5(5) 3_655 3_655 ?
N1 Ru1 N3 88.5(5) . . ?
N1 Ru1 N3 170.6(6) . 3_655 ?
N1 Ru1 N3 170.6(6) 3_655 . ?
N1 Ru1 N1 89.9(7) . 3_655 ?
O1 N5 Ru1 174.9(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3C Cl3 0.86 2.55 3.366(15) 159.3 5_445 yes
N1 H1A Cl2 0.86 2.53 3.343(15) 156.9 . yes
N1 H1C Cl2 0.86 2.81 3.324(14) 119.7 4_565 yes
N1 H1C F1 0.86 2.15 2.876(17) 142.2 2_665 yes

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_kpy300_150k_s3
_database_code_depnum_ccdc_archive 'CCDC 2016495'
loop_
_audit_author_name
_audit_author_address
'Vladislav Komarov'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2020-02-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Pd, F H12 N5 O Ru'
_chemical_formula_sum            'Cl4 H12 F N5 O Pd Ru'
_chemical_formula_weight         466.42
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.1541(3)
_cell_length_b                   17.4696(10)
_cell_length_c                   8.1730(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1164.23(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4354
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      3.42
_shelx_estimated_absorpt_T_max   0.929
_shelx_estimated_absorpt_T_min   0.568
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8212.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 2.00 -1.00 0.2540
2.00 -2.00 1.00 0.2010
1.00 1.00 2.00 0.3050
-1.00 -2.00 -2.00 0.2370
1.00 -1.00 1.00 0.2110
1.00 2.00 0.00 0.2320
-1.00 -2.00 0.00 0.1910
0.00 2.00 -1.00 0.2260
-2.00 -1.00 -1.00 0.2570
-1.00 2.00 -2.00 0.2340
1.00 -2.00 2.00 0.1830
0.00 -1.00 1.00 0.1720
2.00 2.00 -1.00 0.2040
-2.00 -2.00 1.00 0.1790
1.00 2.00 -2.00 0.2080
-1.00 -2.00 2.00 0.1620
2.00 0.00 1.00 0.2940
-2.00 0.00 -1.00 0.2790
0.00 1.00 -2.00 0.2260
0.00 -1.00 2.00 0.1840
1.00 1.00 -2.00 0.1940
-1.00 -1.00 2.00 0.1670
1.00 0.00 0.00 0.1940
-1.00 0.00 0.00 0.1890
2.00 0.00 -1.00 0.1090
-2.00 0.00 1.00 0.1390
1.00 0.00 -1.00 0.1560
-1.00 0.00 1.00 0.1690
2.00 -1.00 -1.00 0.1510
-2.00 1.00 1.00 0.1660
1.00 -1.00 -2.00 0.1820
-1.00 1.00 2.00 0.2100
2.00 -2.00 -1.00 0.1810
-2.00 2.00 1.00 0.1710
1.00 -2.00 -2.00 0.1590
-1.00 2.00 2.00 0.2100
0.00 2.00 1.00 0.2450

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.635
_diffrn_reflns_theta_min         2.332
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                1671
_reflns_number_total             1750
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Flack x determined using 749 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_coef       0.00045(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1750
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0200
_refine_ls_restrained_S_all      1.053
_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)+(0.0122P)²+0.8369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0359
_refine_ls_wR_factor_ref         0.0371
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2.a Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pd1 Pd 1.0000 0.37753(2) 0.68989(3) 0.01045(13) Uani 1 2 d S T P . .
Ru1 Ru 0.5000 0.38019(2) 0.22640(5) 0.00781(12) Uani 1 2 d S T P . .
Cl3 Cl 1.0000 0.32872(8) 0.42278(18) 0.0153(3) Uani 1 2 d S T P . .
Cl1 Cl 1.0000 0.43208(8) 0.94768(17) 0.0148(3) Uani 1 2 d S T P . .
Cl2 Cl 0.71867(11) 0.37044(6) 0.69560(13) 0.0162(2) Uani 1 1 d . . . . .
F1 F 0.5000 0.45459(18) 0.0505(4) 0.0134(7) Uani 1 2 d S T P . .
O1 O 0.5000 0.2617(2) 0.4705(5) 0.0170(10) Uani 1 2 d S T P . .
N5 N 0.5000 0.3112(3) 0.3779(6) 0.0094(9) Uani 1 2 d S T P . .
N3 N 0.3149(4) 0.32449(19) 0.0931(4) 0.0136(7) Uani 1 1 d . . . . .
H3A H 0.3151 0.3419 -0.0119 0.016 Uiso 1 1 calc R U . . .
H3B H 0.2158 0.3343 0.1397 0.016 Uiso 1 1 calc R U . . .
H3C H 0.3336 0.2731 0.0936 0.016 Uiso 1 1 calc R U . . .
N1 N 0.6809(4) 0.44920(18) 0.3313(4) 0.0130(7) Uani 1 1 d . . . . .
H1A H 0.7052 0.4884 0.2621 0.016 Uiso 1 1 calc R U . . .
H1B H 0.7727 0.4208 0.3496 0.016 Uiso 1 1 calc R U . . .
H1C H 0.6437 0.4684 0.4279 0.016 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
Pd1 Cl3 2.3437(15) . ?
Pd1 Cl1 2.3124(14) . ?
Pd1 Cl2 2.2978(9) 4_755 ?
Pd1 Cl2 2.2978(9) . ?
Ru1 F1 1.938(3) . ?
Ru1 N5 1.728(5) . ?
Ru1 N3 2.101(3) 4_655 ?
Ru1 N3 2.101(3) . ?
Ru1 N1 2.089(3) 4_655 ?
Ru1 N1 2.089(3) . ?
O1 N5 1.149(5) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?

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
Cl1 Pd1 Cl3 177.00(6) . . ?
Cl2 Pd1 Cl3 89.96(3) . . ?
Cl2 Pd1 Cl3 89.96(3) 4_755 . ?
Cl2 Pd1 Cl1 90.21(3) 4_755 . ?
Cl2 Pd1 Cl1 90.21(3) . . ?
Cl2 Pd1 Cl2 173.40(6) 4_755 . ?
F1 Ru1 N3 85.75(12) . . ?
F1 Ru1 N3 85.75(12) . 4_655 ?
F1 Ru1 N1 85.26(12) . 4_655 ?
F1 Ru1 N1 85.26(12) . . ?
N5 Ru1 F1 177.90(18) . . ?
N5 Ru1 N3 92.79(14) . . ?
N5 Ru1 N3 92.79(14) . 4_655 ?
N5 Ru1 N1 96.23(14) . . ?
N5 Ru1 N1 96.23(14) . 4_655 ?
N3 Ru1 N3 91.88(18) 4_655 . ?
N1 Ru1 N3 170.95(14) 4_655 4_655 ?
N1 Ru1 N3 170.96(14) . . ?
N1 Ru1 N3 88.44(13) 4_655 . ?
N1 Ru1 N3 88.44(13) . 4_655 ?
N1 Ru1 N1 89.84(19) . 4_655 ?
O1 N5 Ru1 175.4(4) . . ?
Ru1 N3 H3A 109.5 . . ?
Ru1 N3 H3B 109.5 . . ?
Ru1 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Ru1 N1 H1A 109.5 . . ?
Ru1 N1 H1B 109.5 . . ?
Ru1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_ccu_art_m_a4_f_clo4_3_m4_0m
_database_code_depnum_ccdc_archive 'CCDC 2016497'
loop_
_audit_author_name
_audit_author_address
'Vladislav Komarov'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2020-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F H12 N5 O Ru, 2(Cl O4)'
_chemical_formula_sum            'Cl2 H12 F N5 O9 Ru'
_chemical_formula_weight         417.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0038(5)
_cell_length_b                   11.8995(5)
_cell_length_c                   13.8054(8)
_cell_angle_alpha                70.720(2)
_cell_angle_beta                 86.091(2)
_cell_angle_gamma                88.040(2)
_cell_volume                     1238.12(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      3.07
_shelx_estimated_absorpt_T_max   0.933
_shelx_estimated_absorpt_T_min   0.844
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.746542
_exptl_absorpt_correction_T_min  0.603565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 46278 reflections, Rint = 0.0373
 (30050 with I > 3sig(I), Rint = 0.0334)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24099
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.157
_diffrn_reflns_theta_min         1.968
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                18249
_reflns_number_total             24099
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         24099
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.080
_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)+(0.0530P)²+0.1449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5840(6)
 0.4160(6)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3.a Idealised Me refined as rotating group:
 N7(H7A,H7B,H7C), N8(H8A,H8B,H8C), N1(H1A,H1B,H1C), N6(H6A,H6B,H6C), N4(H4A,
 H4B,H4C), N3(H3A,H3B,H3C), N2(H2A,H2B,H2C), N9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.42956(3) 0.74277(2) 0.44096(2) 0.01265(6) Uani 1 1 d . . . . .
Ru2 Ru 0.93715(3) 0.72848(2) 0.94374(2) 0.01271(6) Uani 1 1 d . . . . .
Cl2 Cl 0.48976(10) 0.83798(6) 0.72157(6) 0.01647(14) Uani 1 1 d . . . . .
Cl4 Cl 1.43999(10) 0.63344(7) 1.14041(6) 0.01808(15) Uani 1 1 d . . . . .
Cl3 Cl 0.94893(10) 0.59577(6) 0.63776(6) 0.01660(15) Uani 1 1 d . . . . .
Cl1 Cl -0.04411(10) 0.88871(6) 0.22628(6) 0.01811(15) Uani 1 1 d . . . . .
F2 F 1.0916(2) 0.60519(14) 0.92955(14) 0.0170(4) Uani 1 1 d . . . . .
F1 F 0.5655(2) 0.62209(15) 0.40787(14) 0.0190(4) Uani 1 1 d . . . . .
O11 O 1.0642(3) 0.5069(2) 0.6224(2) 0.0276(6) Uani 1 1 d . . . . .
O7 O 0.6272(3) 0.7636(2) 0.70323(19) 0.0237(5) Uani 1 1 d . . . . .
O6 O -0.1775(3) 0.9666(2) 0.24350(19) 0.0257(5) Uani 1 1 d . . . . .
O12 O 0.9208(3) 0.5777(2) 0.74540(18) 0.0274(6) Uani 1 1 d . . . . .
O18 O 1.2912(3) 0.6806(2) 1.1787(2) 0.0297(6) Uani 1 1 d . . . . .
O2 O 0.7133(3) 0.9142(2) 0.9652(2) 0.0266(6) Uani 1 1 d . . . . .
O1 O 0.2172(3) 0.9226(2) 0.4842(2) 0.0278(6) Uani 1 1 d . . . . .
O17 O 1.4180(3) 0.6384(2) 1.03642(18) 0.0285(6) Uani 1 1 d . . . . .
N7 N 1.1531(3) 0.8180(2) 0.9556(2) 0.0171(5) Uani 1 1 d . . . . .
H7A H 1.170215 0.882189 0.897863 0.021 Uiso 1 1 calc GR . . . .
H7B H 1.243199 0.767763 0.962686 0.021 Uiso 1 1 calc GR . . . .
H7C H 1.139319 0.842699 1.011420 0.021 Uiso 1 1 calc GR . . . .
O14 O 1.0166(3) 0.7129(2) 0.5869(2) 0.0319(6) Uani 1 1 d . . . . .
O16 O 1.5807(3) 0.7052(2) 1.1410(2) 0.0344(6) Uani 1 1 d . . . . .
O13 O 0.7931(3) 0.5875(2) 0.5952(2) 0.0267(6) Uani 1 1 d . . . . .
N5 N 0.3031(3) 0.8517(2) 0.4682(2) 0.0162(5) Uani 1 1 d . . . . .
O3 O -0.0833(4) 0.7678(2) 0.2833(2) 0.0401(7) Uani 1 1 d . . . . .
N8 N 0.9673(4) 0.8033(2) 0.7829(2) 0.0175(5) Uani 1 1 d . . . . .
H8A H 0.873891 0.790134 0.754357 0.021 Uiso 1 1 calc GR . . . .
H8B H 1.057664 0.769157 0.759497 0.021 Uiso 1 1 calc GR . . . .
H8C H 0.983337 0.883082 0.765307 0.021 Uiso 1 1 calc GR . . . .
O8 O 0.4763(4) 0.9413(2) 0.6319(2) 0.0335(7) Uani 1 1 d . . . . .
O4 O 0.1084(3) 0.9207(2) 0.2599(2) 0.0341(6) Uani 1 1 d . . . . .
N1 N 0.4186(3) 0.6221(2) 0.5914(2) 0.0163(5) Uani 1 1 d . . . . .
H1A H 0.420765 0.546381 0.589434 0.020 Uiso 1 1 calc GR . . . .
H1B H 0.322252 0.634660 0.625497 0.020 Uiso 1 1 calc GR . . . .
H1C H 0.508090 0.632956 0.624473 0.020 Uiso 1 1 calc GR . . . .
N6 N 0.9320(4) 0.6326(2) 1.1018(2) 0.0187(6) Uani 1 1 d . . . . .
H6A H 0.936281 0.553158 1.111254 0.022 Uiso 1 1 calc GR . . . .
H6B H 0.835889 0.650357 1.133109 0.022 Uiso 1 1 calc GR . . . .
H6C H 1.021767 0.652651 1.129455 0.022 Uiso 1 1 calc GR . . . .
N10 N 0.8008(3) 0.8400(2) 0.9565(2) 0.0167(5) Uani 1 1 d . . . . .
O5 O -0.0238(4) 0.9059(3) 0.1184(2) 0.0378(7) Uani 1 1 d . . . . .
N4 N 0.2290(3) 0.6545(2) 0.4098(2) 0.0179(5) Uani 1 1 d . . . . .
H4A H 0.259656 0.628493 0.356073 0.022 Uiso 1 1 calc GR . . . .
H4B H 0.139979 0.705449 0.393511 0.022 Uiso 1 1 calc GR . . . .
H4C H 0.200167 0.591223 0.466279 0.022 Uiso 1 1 calc GR . . . .
N3 N 0.4667(4) 0.8410(2) 0.2836(2) 0.0181(5) Uani 1 1 d . . . . .
H3A H 0.541061 0.801549 0.253173 0.022 Uiso 1 1 calc GR . . . .
H3B H 0.507720 0.913884 0.276420 0.022 Uiso 1 1 calc GR . . . .
H3C H 0.367457 0.849972 0.253293 0.022 Uiso 1 1 calc GR . . . .
N2 N 0.6559(3) 0.8119(2) 0.4644(2) 0.0171(5) Uani 1 1 d . . . . .
H2A H 0.669404 0.886932 0.419184 0.021 Uiso 1 1 calc GR . . . .
H2B H 0.742719 0.764747 0.454309 0.021 Uiso 1 1 calc GR . . . .
H2C H 0.653621 0.813853 0.529794 0.021 Uiso 1 1 calc GR . . . .
O9 O 0.3383(3) 0.7724(2) 0.7402(3) 0.0406(7) Uani 1 1 d . . . . .
N9 N 0.7507(3) 0.6151(2) 0.9306(2) 0.0172(5) Uani 1 1 d . . . . .
H9A H 0.745415 0.621024 0.863463 0.021 Uiso 1 1 calc GR . . . .
H9B H 0.649979 0.636546 0.954453 0.021 Uiso 1 1 calc GR . . . .
H9C H 0.775850 0.538625 0.968243 0.021 Uiso 1 1 calc GR . . . .
O10 O 0.5203(4) 0.8738(3) 0.8078(2) 0.0414(7) Uani 1 1 d . . . . .
O15 O 1.4685(4) 0.5141(2) 1.2007(2) 0.0445(8) 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 F1 1.9269(18) . ?
Ru1 N5 1.739(3) . ?
Ru1 N1 2.097(2) . ?
Ru1 N4 2.091(3) . ?
Ru1 N3 2.105(3) . ?
Ru1 N2 2.103(3) . ?
Ru2 F2 1.9369(17) . ?
Ru2 N7 2.104(3) . ?
Ru2 N8 2.101(3) . ?
Ru2 N6 2.100(3) . ?
Ru2 N10 1.736(3) . ?
Ru2 N9 2.102(3) . ?
Cl2 O7 1.449(2) . ?
Cl2 O8 1.435(2) . ?
Cl2 O9 1.426(3) . ?
Cl2 O10 1.428(3) . ?
Cl4 O18 1.441(2) . ?
Cl4 O17 1.440(2) . ?
Cl4 O16 1.439(3) . ?
Cl4 O15 1.409(3) . ?
Cl3 O11 1.438(2) . ?
Cl3 O12 1.432(3) . ?
Cl3 O14 1.442(2) . ?
Cl3 O13 1.435(2) . ?
Cl1 O6 1.449(2) . ?
Cl1 O3 1.427(2) . ?
Cl1 O4 1.441(3) . ?
Cl1 O5 1.433(3) . ?
O2 N10 1.140(3) . ?
O1 N5 1.139(3) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?

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
F1 Ru1 N1 84.92(9) . . ?
F1 Ru1 N4 84.61(10) . . ?
F1 Ru1 N3 85.06(9) . . ?
F1 Ru1 N2 86.12(9) . . ?
N5 Ru1 F1 178.38(10) . . ?
N5 Ru1 N1 96.00(11) . . ?
N5 Ru1 N4 94.08(12) . . ?
N5 Ru1 N3 94.02(12) . . ?
N5 Ru1 N2 95.18(12) . . ?
N1 Ru1 N3 169.98(10) . . ?
N1 Ru1 N2 91.22(10) . . ?
N4 Ru1 N1 88.74(10) . . ?
N4 Ru1 N3 90.38(10) . . ?
N4 Ru1 N2 170.70(10) . . ?
N2 Ru1 N3 88.03(10) . . ?
F2 Ru2 N7 85.18(9) . . ?
F2 Ru2 N8 86.06(9) . . ?
F2 Ru2 N6 85.04(9) . . ?
F2 Ru2 N9 84.82(9) . . ?
N8 Ru2 N7 89.07(10) . . ?
N8 Ru2 N9 90.74(11) . . ?
N6 Ru2 N7 90.46(11) . . ?
N6 Ru2 N8 171.10(11) . . ?
N6 Ru2 N9 88.18(10) . . ?
N10 Ru2 F2 179.30(10) . . ?
N10 Ru2 N7 94.13(12) . . ?
N10 Ru2 N8 93.89(12) . . ?
N10 Ru2 N6 95.01(12) . . ?
N10 Ru2 N9 95.88(12) . . ?
N9 Ru2 N7 169.98(10) . . ?
O8 Cl2 O7 108.95(16) . . ?
O9 Cl2 O7 108.93(15) . . ?
O9 Cl2 O8 109.12(18) . . ?
O9 Cl2 O10 110.47(19) . . ?
O10 Cl2 O7 109.73(16) . . ?
O10 Cl2 O8 109.61(17) . . ?
O17 Cl4 O18 108.74(15) . . ?
O16 Cl4 O18 109.17(15) . . ?
O16 Cl4 O17 109.07(17) . . ?
O15 Cl4 O18 110.77(18) . . ?
O15 Cl4 O17 108.78(17) . . ?
O15 Cl4 O16 110.27(18) . . ?
O11 Cl3 O14 109.86(15) . . ?
O12 Cl3 O11 109.88(15) . . ?
O12 Cl3 O14 109.22(15) . . ?
O12 Cl3 O13 109.48(16) . . ?
O13 Cl3 O11 109.46(14) . . ?
O13 Cl3 O14 108.92(15) . . ?
O3 Cl1 O6 109.89(16) . . ?
O3 Cl1 O4 109.76(17) . . ?
O3 Cl1 O5 110.79(18) . . ?
O4 Cl1 O6 108.37(15) . . ?
O5 Cl1 O6 108.80(16) . . ?
O5 Cl1 O4 109.18(17) . . ?
Ru2 N7 H7A 109.5 . . ?
Ru2 N7 H7B 109.5 . . ?
Ru2 N7 H7C 109.5 . . ?
H7A N7 H7B 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
O1 N5 Ru1 178.1(3) . . ?
Ru2 N8 H8A 109.5 . . ?
Ru2 N8 H8B 109.5 . . ?
Ru2 N8 H8C 109.5 . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
Ru1 N1 H1A 109.5 . . ?
Ru1 N1 H1B 109.5 . . ?
Ru1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Ru2 N6 H6A 109.5 . . ?
Ru2 N6 H6B 109.5 . . ?
Ru2 N6 H6C 109.5 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
O2 N10 Ru2 178.9(3) . . ?
Ru1 N4 H4A 109.5 . . ?
Ru1 N4 H4B 109.5 . . ?
Ru1 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
Ru1 N3 H3A 109.5 . . ?
Ru1 N3 H3B 109.5 . . ?
Ru1 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Ru1 N2 H2A 109.5 . . ?
Ru1 N2 H2B 109.5 . . ?
Ru1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Ru2 N9 H9A 109.5 . . ?
Ru2 N9 H9B 109.5 . . ?
Ru2 N9 H9C 109.5 . . ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5840(6)
2 0.4160(6)

