# 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_3i
_database_code_depnum_ccdc_archive 'CCDC 1537314'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C23 H17 Br Cl2 N4 Ru, F6 P, 2(C2 H3 N)'
_chemical_formula_sum            'C27 H23 Br Cl2 F6 N6 P Ru'
_chemical_formula_weight         828.35
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_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                   9.9381(6)
_cell_length_b                   9.8000(6)
_cell_length_c                   31.5878(19)
_cell_angle_alpha                90
_cell_angle_beta                 98.325(3)
_cell_angle_gamma                90
_cell_volume                     3044.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9203
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      35.04
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1636
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_T_max  0.7470

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_number            171898
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         35.84
_diffrn_reflns_theta_full        35.84
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             14207
_reflns_number_gt                12450
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0194P)²+3.5713P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         14207
_refine_ls_number_parameters     456
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.104

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C16 C 0.35055(16) 0.61111(17) 0.28966(5) 0.0174(3) Uani 1 1 d . . .
C17 C 0.25339(19) 0.6678(2) 0.25489(6) 0.0239(3) Uani 1 1 d . . .
H17A H 0.284 0.6478 0.2274 0.036 Uiso 1 1 calc R . .
H17B H 0.2473 0.7668 0.2585 0.036 Uiso 1 1 calc R . .
H17C H 0.1638 0.6267 0.2554 0.036 Uiso 1 1 calc R . .
C1 C 0.45782(15) 0.65846(15) 0.42471(5) 0.0150(3) Uani 1 1 d . . .
H1 H 0.3907 0.6851 0.4017 0.018 Uiso 1 1 calc R . .
C2 C 0.45432(16) 0.71415(16) 0.46500(5) 0.0163(3) Uani 1 1 d . . .
H2 H 0.3849 0.7768 0.4695 0.02 Uiso 1 1 calc R . .
C3 C 0.55370(16) 0.67690(15) 0.49852(5) 0.0153(3) Uani 1 1 d . . .
H3 H 0.5536 0.7146 0.5262 0.018 Uiso 1 1 calc R . .
C4 C 0.65352(15) 0.58375(15) 0.49119(5) 0.0129(2) Uani 1 1 d . . .
H4 H 0.723 0.5581 0.5137 0.016 Uiso 1 1 calc R . .
C5 C 0.65023(14) 0.52894(14) 0.45067(5) 0.0113(2) Uani 1 1 d . . .
C6 C 0.74538(14) 0.42297(14) 0.43993(4) 0.0112(2) Uani 1 1 d . . .
C7 C 0.85164(14) 0.36378(15) 0.46737(4) 0.0119(2) Uani 1 1 d . . .
H7 H 0.8702 0.3916 0.4964 0.014 Uiso 1 1 calc R . .
C8 C 0.93101(14) 0.26246(15) 0.45155(4) 0.0116(2) Uani 1 1 d . . .
C9 C 0.90122(14) 0.22533(15) 0.40830(4) 0.0122(2) Uani 1 1 d . . .
H9 H 0.9529 0.1563 0.397 0.015 Uiso 1 1 calc R . .
C10 C 0.79630(14) 0.28950(15) 0.38218(4) 0.0114(2) Uani 1 1 d . . .
C11 C 0.75530(14) 0.26607(15) 0.33588(4) 0.0123(2) Uani 1 1 d . . .
C12 C 0.82148(16) 0.17799(17) 0.31169(5) 0.0167(3) Uani 1 1 d . . .
H12 H 0.8983 0.1276 0.3246 0.02 Uiso 1 1 calc R . .
C13 C 0.77467(17) 0.16373(18) 0.26835(5) 0.0193(3) Uani 1 1 d . . .
H13 H 0.8199 0.1043 0.2512 0.023 Uiso 1 1 calc R . .
C14 C 0.66131(17) 0.23691(18) 0.25018(5) 0.0179(3) Uani 1 1 d . . .
H14 H 0.6265 0.2269 0.2207 0.021 Uiso 1 1 calc R . .
C15 C 0.60003(16) 0.32474(17) 0.27588(5) 0.0153(3) Uani 1 1 d . . .
H15 H 0.5228 0.3756 0.2635 0.018 Uiso 1 1 calc R . .
C18 C 1.04465(14) 0.19463(15) 0.47916(5) 0.0119(2) Uani 1 1 d . . .
C19 C 1.04964(15) 0.18759(16) 0.52359(5) 0.0147(3) Uani 1 1 d . . .
H19 H 0.9807 0.2305 0.5368 0.018 Uiso 1 1 calc R . .
C20 C 1.15485(15) 0.11813(16) 0.54869(5) 0.0155(3) Uani 1 1 d . . .
H20 H 1.1586 0.1146 0.5789 0.019 Uiso 1 1 calc R . .
C21 C 1.25381(14) 0.05423(15) 0.52903(5) 0.0128(2) Uani 1 1 d . . .
C22 C 1.25241(15) 0.06155(15) 0.48511(5) 0.0135(2) Uani 1 1 d . . .
H22 H 1.3217 0.0185 0.4721 0.016 Uiso 1 1 calc R . .
C23 C 1.14847(15) 0.13256(16) 0.46050(5) 0.0134(2) Uani 1 1 d . . .
H23 H 1.1477 0.1392 0.4305 0.016 Uiso 1 1 calc R . .
C24 C 0.9696(2) 0.4186(2) 0.21426(6) 0.0259(3) Uani 1 1 d . . .
C25 C 0.9310(2) 0.4489(2) 0.16915(7) 0.0294(4) Uani 1 1 d . . .
H25A H 0.9623 0.5407 0.1631 0.044 Uiso 1 1 calc R . .
H25B H 0.8318 0.4443 0.1619 0.044 Uiso 1 1 calc R . .
H25C H 0.9728 0.3821 0.152 0.044 Uiso 1 1 calc R . .
C26 C 0.39726(18) 1.00206(18) 0.10630(6) 0.0203(3) Uani 1 1 d . . .
C27 C 0.41674(19) 0.9539(2) 0.15036(6) 0.0226(3) Uani 1 1 d . . .
H27A H 0.4119 0.854 0.1507 0.034 Uiso 1 1 calc R . .
H27B H 0.3455 0.9918 0.1653 0.034 Uiso 1 1 calc R . .
H27C H 0.506 0.9835 0.1647 0.034 Uiso 1 1 calc R . .
N4 N 0.42477(14) 0.56463(14) 0.31671(4) 0.0164(2) Uani 1 1 d . . .
N1 N 0.55325(13) 0.56816(13) 0.41750(4) 0.0124(2) Uani 1 1 d . . .
N2 N 0.72070(12) 0.38421(12) 0.39868(4) 0.01074(19) Uani 1 1 d . . .
N3 N 0.64598(13) 0.34049(13) 0.31762(4) 0.0126(2) Uani 1 1 d . . .
N5 N 1.0010(2) 0.3957(2) 0.24972(6) 0.0370(4) Uani 1 1 d . . .
N6 N 0.38232(19) 1.03867(19) 0.07161(5) 0.0282(3) Uani 1 1 d . . .
P1 P 0.35566(5) 0.41819(5) 0.151507(14) 0.01978(8) Uani 1 1 d DU . .
F1 F 0.2189(5) 0.4089(8) 0.1691(2) 0.0597(15) Uani 0.570(10) 1 d PDU A 1
F2 F 0.4316(6) 0.4534(5) 0.19891(13) 0.0351(9) Uani 0.570(10) 1 d PDU A 1
F3 F 0.5038(5) 0.4240(4) 0.13504(17) 0.0382(9) Uani 0.570(10) 1 d PDU A 1
F4 F 0.2901(7) 0.3764(5) 0.10507(12) 0.0564(14) Uani 0.570(10) 1 d PDU A 1
F5 F 0.3883(6) 0.2580(5) 0.16337(17) 0.0390(10) Uani 0.570(10) 1 d PDU A 1
F6 F 0.3397(10) 0.5743(7) 0.1418(3) 0.0348(15) Uani 0.570(10) 1 d PDU A 1
F1' F 0.2416(7) 0.4351(6) 0.1833(2) 0.0364(12) Uani 0.430(10) 1 d PDU A 2
F2' F 0.4667(7) 0.4281(8) 0.1917(2) 0.0427(15) Uani 0.430(10) 1 d PDU A 2
F3' F 0.4601(8) 0.4107(6) 0.1197(2) 0.0419(14) Uani 0.430(10) 1 d PDU A 2
F4' F 0.2310(6) 0.4221(7) 0.11160(17) 0.0458(14) Uani 0.430(10) 1 d PDU A 2
F5' F 0.3387(8) 0.2602(6) 0.1546(2) 0.0348(12) Uani 0.430(10) 1 d PDU A 2
F6' F 0.3566(11) 0.5846(7) 0.1478(4) 0.0207(11) Uani 0.430(10) 1 d PDU A 2
Cl2 Cl 0.42048(4) 0.30492(4) 0.374913(13) 0.01781(7) Uani 1 1 d . . .
Cl1 Cl 0.73025(4) 0.63539(4) 0.346244(12) 0.01799(7) Uani 1 1 d . . .
Br1 Br 1.394020(15) -0.046514(16) 0.562219(5) 0.01593(3) Uani 1 1 d . . .
Ru1 Ru 0.573931(11) 0.471543(12) 0.360400(4) 0.01088(3) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C16 N4 1.140(2) . ?
C16 C17 1.463(2) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C1 N1 1.3406(19) . ?
C1 C2 1.390(2) . ?
C1 H1 0.95 . ?
C2 C3 1.388(2) . ?
C2 H2 0.95 . ?
C3 C4 1.392(2) . ?
C3 H3 0.95 . ?
C4 C5 1.384(2) . ?
C4 H4 0.95 . ?
C5 N1 1.3718(19) . ?
C5 C6 1.477(2) . ?
C6 N2 1.3452(18) . ?
C6 C7 1.392(2) . ?
C7 C8 1.404(2) . ?
C7 H7 0.95 . ?
C8 C9 1.403(2) . ?
C8 C18 1.481(2) . ?
C9 C10 1.384(2) . ?
C9 H9 0.95 . ?
C10 N2 1.3458(18) . ?
C10 C11 1.478(2) . ?
C11 N3 1.3651(19) . ?
C11 C12 1.381(2) . ?
C12 C13 1.388(2) . ?
C12 H12 0.95 . ?
C13 C14 1.388(2) . ?
C13 H13 0.95 . ?
C14 C15 1.384(2) . ?
C14 H14 0.95 . ?
C15 N3 1.3402(19) . ?
C15 H15 0.95 . ?
C18 C19 1.399(2) . ?
C18 C23 1.399(2) . ?
C19 C20 1.395(2) . ?
C19 H19 0.95 . ?
C20 C21 1.386(2) . ?
C20 H20 0.95 . ?
C21 C22 1.387(2) . ?
C21 Br1 1.8953(14) . ?
C22 C23 1.387(2) . ?
C22 H22 0.95 . ?
C23 H23 0.95 . ?
C24 N5 1.141(3) . ?
C24 C25 1.452(3) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 N6 1.142(2) . ?
C26 C27 1.456(2) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
N4 Ru1 2.0837(14) . ?
N1 Ru1 2.0735(13) . ?
N2 Ru1 1.9523(12) . ?
N3 Ru1 2.0661(13) . ?
P1 F1 1.545(5) . ?
P1 F3' 1.547(4) . ?
P1 F2' 1.560(6) . ?
P1 F5' 1.562(5) . ?
P1 F6 1.564(7) . ?
P1 F4 1.571(3) . ?
P1 F2 1.614(4) . ?
P1 F1' 1.628(5) . ?
P1 F3 1.632(4) . ?
P1 F4' 1.635(4) . ?
P1 F5 1.635(5) . ?
P1 F6' 1.635(7) . ?
Cl2 Ru1 2.3248(4) . ?
Cl1 Ru1 2.3223(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 C16 C17 178.65(19) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C1 C2 121.80(14) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.07(14) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.40(14) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.11(14) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.16(13) . . ?
N1 C5 C6 115.09(12) . . ?
C4 C5 C6 123.73(13) . . ?
N2 C6 C7 120.06(13) . . ?
N2 C6 C5 112.83(12) . . ?
C7 C6 C5 127.10(13) . . ?
C6 C7 C8 119.18(13) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 118.66(13) . . ?
C9 C8 C18 119.50(13) . . ?
C7 C8 C18 121.84(13) . . ?
C10 C9 C8 119.81(13) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
N2 C10 C9 119.83(13) . . ?
N2 C10 C11 113.64(12) . . ?
C9 C10 C11 126.54(13) . . ?
N3 C11 C12 120.93(13) . . ?
N3 C11 C10 115.06(12) . . ?
C12 C11 C10 124.01(13) . . ?
C11 C12 C13 119.36(14) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 119.48(15) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 118.60(14) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
N3 C15 C14 122.19(14) . . ?
N3 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C19 C18 C23 118.68(13) . . ?
C19 C18 C8 121.75(13) . . ?
C23 C18 C8 119.54(13) . . ?
C20 C19 C18 120.61(13) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C21 C20 C19 119.21(14) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 121.30(13) . . ?
C20 C21 Br1 120.00(11) . . ?
C22 C21 Br1 118.70(11) . . ?
C23 C22 C21 119.04(13) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C18 121.11(13) . . ?
C22 C23 H23 119.4 . . ?
C18 C23 H23 119.4 . . ?
N5 C24 C25 179.3(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 179.4(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C16 N4 Ru1 173.01(14) . . ?
C1 N1 C5 119.42(13) . . ?
C1 N1 Ru1 127.66(11) . . ?
C5 N1 Ru1 112.91(9) . . ?
C6 N2 C10 122.42(12) . . ?
C6 N2 Ru1 119.42(10) . . ?
C10 N2 Ru1 118.13(10) . . ?
C15 N3 C11 119.41(13) . . ?
C15 N3 Ru1 127.88(10) . . ?
C11 N3 Ru1 112.69(9) . . ?
F1 P1 F3' 160.0(3) . . ?
F1 P1 F2' 105.4(3) . . ?
F3' P1 F2' 94.0(3) . . ?
F1 P1 F5' 79.1(3) . . ?
F3' P1 F5' 94.7(3) . . ?
F2' P1 F5' 94.7(3) . . ?
F1 P1 F6 93.4(4) . . ?
F3' P1 F6 88.7(4) . . ?
F2' P1 F6 97.9(4) . . ?
F5' P1 F6 166.7(4) . . ?
F1 P1 F4 93.1(2) . . ?
F3' P1 F4 66.9(3) . . ?
F2' P1 F4 157.7(3) . . ?
F5' P1 F4 76.4(3) . . ?
F6 P1 F4 93.2(4) . . ?
F1 P1 F2 89.8(3) . . ?
F3' P1 F2 110.2(3) . . ?
F5' P1 F2 101.2(3) . . ?
F6 P1 F2 89.6(4) . . ?
F4 P1 F2 175.9(3) . . ?
F3' P1 F1' 176.2(3) . . ?
F2' P1 F1' 88.0(3) . . ?
F5' P1 F1' 88.4(3) . . ?
F6 P1 F1' 87.8(5) . . ?
F4 P1 F1' 111.8(3) . . ?
F2 P1 F1' 71.3(3) . . ?
F1 P1 F3 177.1(3) . . ?
F2' P1 F3 72.1(3) . . ?
F5' P1 F3 99.5(3) . . ?
F6 P1 F3 88.5(4) . . ?
F4 P1 F3 89.0(2) . . ?
F2 P1 F3 88.0(2) . . ?
F1' P1 F3 159.0(2) . . ?
F1 P1 F4' 70.8(3) . . ?
F3' P1 F4' 90.3(3) . . ?
F2' P1 F4' 173.7(3) . . ?
F5' P1 F4' 89.7(3) . . ?
F6 P1 F4' 77.4(4) . . ?
F2 P1 F4' 155.6(3) . . ?
F1' P1 F4' 87.5(3) . . ?
F3 P1 F4' 111.8(2) . . ?
F1 P1 F5 91.0(3) . . ?
F3' P1 F5 88.5(3) . . ?
F2' P1 F5 77.3(3) . . ?
F6 P1 F5 174.3(4) . . ?
F4 P1 F5 90.3(2) . . ?
F2 P1 F5 86.7(2) . . ?
F1' P1 F5 95.1(3) . . ?
F3 P1 F5 87.0(3) . . ?
F4' P1 F5 107.6(2) . . ?
F1 P1 F6' 95.7(5) . . ?
F3' P1 F6' 89.4(5) . . ?
F2' P1 F6' 89.2(4) . . ?
F5' P1 F6' 174.2(5) . . ?
F4 P1 F6' 101.5(4) . . ?
F2 P1 F6' 81.2(4) . . ?
F1' P1 F6' 87.4(5) . . ?
F3 P1 F6' 85.8(4) . . ?
F4' P1 F6' 86.2(4) . . ?
F5 P1 F6' 166.1(4) . . ?
N2 Ru1 N3 80.44(5) . . ?
N2 Ru1 N1 79.67(5) . . ?
N3 Ru1 N1 160.09(5) . . ?
N2 Ru1 N4 176.58(5) . . ?
N3 Ru1 N4 96.87(5) . . ?
N1 Ru1 N4 103.04(5) . . ?
N2 Ru1 Cl1 87.81(4) . . ?
N3 Ru1 Cl1 89.94(4) . . ?
N1 Ru1 Cl1 90.29(4) . . ?
N4 Ru1 Cl1 90.08(4) . . ?
N2 Ru1 Cl2 91.29(4) . . ?
N3 Ru1 Cl2 89.53(4) . . ?
N1 Ru1 Cl2 89.93(4) . . ?
N4 Ru1 Cl2 90.80(4) . . ?
Cl1 Ru1 Cl2 179.020(15) . . ?
####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1537310'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H15 Cl2 N4 O Ru, Cl, H2 O '
_chemical_formula_sum            'C21 H17 Cl3 N4 O2 Ru '
_chemical_formula_weight         564.81

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'
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'
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'
P P 0.1023 0.0942 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   28.0160(14)
_cell_length_b                   8.6148(5)
_cell_length_c                   20.3292(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4906.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4617
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      21.80

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.990
_shelx_estimated_absorpt_T_min   0.943
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            82713
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_av_R_equivalents  0.1628
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.454
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4494
_reflns_number_gt                3043
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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)+(0.0290P)²+8.8314P] 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         4494
_refine_ls_number_parameters     290
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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
C1 C 0.34338(16) -0.0401(5) 0.4510(2) 0.0187(10) Uani 1 1 d . . . . .
H1 H 0.3136 -0.0099 0.4327 0.022 Uiso 1 1 calc R U . . .
C2 C 0.36201(16) -0.1839(5) 0.4363(2) 0.0230(11) Uani 1 1 d . . . . .
H2 H 0.3452 -0.2519 0.4077 0.028 Uiso 1 1 calc R U . . .
C3 C 0.40492(16) -0.2291(5) 0.4630(2) 0.0231(11) Uani 1 1 d . . . . .
H3 H 0.4180 -0.3281 0.4528 0.028 Uiso 1 1 calc R U . . .
C4 C 0.42891(16) -0.1285(5) 0.5049(2) 0.0200(10) Uani 1 1 d . . . . .
H4 H 0.4584 -0.1582 0.5241 0.024 Uiso 1 1 calc R U . . .
C5 C 0.40941(14) 0.0150(5) 0.5183(2) 0.0154(9) Uani 1 1 d . . . . .
C6 C 0.43130(15) 0.1297(5) 0.5631(2) 0.0153(10) Uani 1 1 d . . . . .
C7 C 0.47252(14) 0.1118(5) 0.59948(19) 0.0145(10) Uani 1 1 d . . . . .
H7 H 0.4903 0.0181 0.5968 0.017 Uiso 1 1 calc R U . . .
C8 C 0.48800(14) 0.2325(5) 0.64043(19) 0.0152(9) Uani 1 1 d . . . . .
C9 C 0.46078(14) 0.3682(5) 0.6447(2) 0.0159(10) Uani 1 1 d . . . . .
H9 H 0.4704 0.4507 0.6728 0.019 Uiso 1 1 calc R U . . .
C10 C 0.41955(15) 0.3805(5) 0.60745(19) 0.0144(9) Uani 1 1 d . . . . .
C11 C 0.38599(14) 0.5119(5) 0.60620(19) 0.0140(9) Uani 1 1 d . . . . .
C12 C 0.39250(15) 0.6490(5) 0.6407(2) 0.0175(10) Uani 1 1 d . . . . .
H12 H 0.4198 0.6625 0.6678 0.021 Uiso 1 1 calc R U . . .
C13 C 0.35886(15) 0.7663(5) 0.6354(2) 0.0214(11) Uani 1 1 d . . . . .
H13 H 0.3636 0.8620 0.6577 0.026 Uiso 1 1 calc R U . . .
C14 C 0.31849(16) 0.7437(5) 0.5977(2) 0.0215(11) Uani 1 1 d . . . . .
H14 H 0.2949 0.8226 0.5944 0.026 Uiso 1 1 calc R U . . .
C15 C 0.31296(15) 0.6040(5) 0.5647(2) 0.0182(10) Uani 1 1 d . . . . .
H15 H 0.2851 0.5871 0.5391 0.022 Uiso 1 1 calc R U . . .
C16 C 0.53317(15) 0.2182(5) 0.67743(19) 0.0185(10) Uani 1 1 d . . . . .
C17 C 0.54913(16) 0.0719(6) 0.6974(2) 0.0264(12) Uani 1 1 d . . . . .
H17 H 0.5301 -0.0172 0.6889 0.032 Uiso 1 1 calc R U . . .
C18 C 0.59220(18) 0.0560(6) 0.7294(2) 0.0358(13) Uani 1 1 d . . . . .
H18 H 0.6027 -0.0436 0.7434 0.043 Uiso 1 1 calc R U . . .
C19 C 0.62016(17) 0.1857(6) 0.7412(2) 0.0319(13) Uani 1 1 d . . . . .
H19 H 0.6502 0.1742 0.7623 0.038 Uiso 1 1 calc R U . . .
C20 C 0.60477(16) 0.3311(6) 0.7227(2) 0.0255(12) Uani 1 1 d . . . . .
H20 H 0.6238 0.4198 0.7317 0.031 Uiso 1 1 calc R U . . .
C21 C 0.56105(15) 0.3478(5) 0.6905(2) 0.0201(10) Uani 1 1 d . . . . .
H21 H 0.5504 0.4479 0.6775 0.024 Uiso 1 1 calc R U . . .
Cl1 Cl 0.27019(4) 0.29774(13) 0.46435(5) 0.0225(3) Uani 1 1 d . . . . .
Cl2 Cl 0.30880(4) 0.17145(12) 0.60791(5) 0.0198(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5000 0.30503(19) 0.2500 0.0304(4) Uani 1 2 d S T P . .
N1 N 0.37010(12) 0.3631(4) 0.44453(17) 0.0143(8) Uani 1 1 d . . . . .
N2 N 0.36676(12) 0.0577(4) 0.49079(16) 0.0148(8) Uani 1 1 d . . . . .
N3 N 0.40638(11) 0.2630(4) 0.56775(16) 0.0142(8) Uani 1 1 d . . . . .
N4 N 0.34604(12) 0.4929(4) 0.56818(15) 0.0147(8) Uani 1 1 d . . . . .
O1 O 0.37937(12) 0.4136(4) 0.39480(16) 0.0329(8) Uani 1 1 d . . . . .
Ru1 Ru 0.34641(2) 0.28237(4) 0.51713(2) 0.01438(10) Uani 1 1 d . . . . .
Cl4 Cl 0.5000 0.5000 0.5000 0.0392(5) Uani 1 2 d S . P . .
O2 O 0.47140(15) 0.2329(5) 0.4054(2) 0.0426(10) Uani 1 1 d D . . . .
H2A H 0.4806(18) 0.308(4) 0.430(2) 0.048(19) Uiso 1 1 d D . . . .
H2B H 0.4783(19) 0.255(6) 0.3656(10) 0.05(2) 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
C1 N2 1.339(5) . ?
C1 C2 1.377(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9500 . ?
C5 N2 1.369(5) . ?
C5 C6 1.477(6) . ?
C6 N3 1.347(5) . ?
C6 C7 1.380(6) . ?
C7 C8 1.401(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.399(6) . ?
C8 C16 1.477(6) . ?
C9 C10 1.386(6) . ?
C9 H9 0.9500 . ?
C10 N3 1.346(5) . ?
C10 C11 1.472(6) . ?
C11 N4 1.370(5) . ?
C11 C12 1.385(6) . ?
C12 C13 1.386(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(6) . ?
C14 H14 0.9500 . ?
C15 N4 1.334(5) . ?
C15 H15 0.9500 . ?
C16 C21 1.388(6) . ?
C16 C17 1.398(6) . ?
C17 C18 1.378(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.396(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
Cl1 Ru1 2.3936(11) . ?
Cl2 Ru1 2.3300(11) . ?
N1 O1 1.131(4) . ?
N1 Ru1 1.761(4) . ?
N2 Ru1 2.088(3) . ?
N3 Ru1 1.977(3) . ?
N4 Ru1 2.089(3) . ?
O2 H2A 0.857(10) . ?
O2 H2B 0.853(10) . ?

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 C1 C2 120.8(4) . . ?
N2 C1 H1 119.6 . . ?
C2 C1 H1 119.6 . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N2 C5 C4 120.4(4) . . ?
N2 C5 C6 115.7(4) . . ?
C4 C5 C6 123.8(4) . . ?
N3 C6 C7 119.4(4) . . ?
N3 C6 C5 113.5(4) . . ?
C7 C6 C5 127.1(4) . . ?
C6 C7 C8 119.6(4) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 C16 120.3(4) . . ?
C7 C8 C16 120.4(4) . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N3 C10 C9 119.9(4) . . ?
N3 C10 C11 113.1(4) . . ?
C9 C10 C11 126.9(4) . . ?
N4 C11 C12 119.7(4) . . ?
N4 C11 C10 116.1(4) . . ?
C12 C11 C10 124.2(4) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 119.8(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 118.9(4) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
N4 C15 C14 121.3(4) . . ?
N4 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C21 C16 C17 119.3(4) . . ?
C21 C16 C8 120.8(4) . . ?
C17 C16 C8 119.8(4) . . ?
C18 C17 C16 120.5(5) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.8(5) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 119.8(4) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C16 C21 C20 120.0(4) . . ?
C16 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
O1 N1 Ru1 170.9(3) . . ?
C1 N2 C5 120.3(4) . . ?
C1 N2 Ru1 127.2(3) . . ?
C5 N2 Ru1 112.5(3) . . ?
C10 N3 C6 122.8(4) . . ?
C10 N3 Ru1 118.8(3) . . ?
C6 N3 Ru1 118.4(3) . . ?
C15 N4 C11 120.8(4) . . ?
C15 N4 Ru1 126.8(3) . . ?
C11 N4 Ru1 112.3(3) . . ?
N1 Ru1 N3 98.58(14) . . ?
N1 Ru1 N2 92.76(14) . . ?
N3 Ru1 N2 79.81(13) . . ?
N1 Ru1 N4 94.33(14) . . ?
N3 Ru1 N4 79.57(13) . . ?
N2 Ru1 N4 158.98(13) . . ?
N1 Ru1 Cl2 174.87(11) . . ?
N3 Ru1 Cl2 86.42(10) . . ?
N2 Ru1 Cl2 86.93(9) . . ?
N4 Ru1 Cl2 87.72(9) . . ?
N1 Ru1 Cl1 86.49(11) . . ?
N3 Ru1 Cl1 174.92(10) . . ?
N2 Ru1 Cl1 100.37(10) . . ?
N4 Ru1 Cl1 99.80(10) . . ?
Cl2 Ru1 Cl1 88.53(4) . . ?
H2A O2 H2B 108(5) . . ?

_refine_diff_density_max         0.508
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.103


####################################################################### 
# 
# 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_2t
_database_code_depnum_ccdc_archive 'CCDC 1537309'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;


#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H15 Cl2 N4 O Ru, F6 P'
_chemical_formula_sum            'C21 H15 Cl2 F6 N4 O P Ru'
_chemical_formula_weight         656.31
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_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                   14.023(6)
_cell_length_b                   7.125(4)
_cell_length_c                   25.620(12)
_cell_angle_alpha                90
_cell_angle_beta                 105.620(17)
_cell_angle_gamma                90
_cell_volume                     2465(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9901
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      27.87
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6954
_exptl_absorpt_correction_T_max  0.7457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.08
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_number            79983
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.9
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             6106
_reflns_number_gt                4705
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0266P)²+3.6991P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6106
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0701
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.106

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1525(2) 0.6372(4) 0.46354(12) 0.0194(6) Uani 1 1 d . . .
H1 H 0.1821 0.6265 0.4344 0.023 Uiso 1 1 calc R . .
C2 C 0.0668(2) 0.7404(4) 0.45615(13) 0.0225(6) Uani 1 1 d . . .
H2 H 0.0382 0.8004 0.4224 0.027 Uiso 1 1 calc R . .
C3 C 0.0226(2) 0.7559(4) 0.49811(13) 0.0215(6) Uani 1 1 d . . .
H3 H -0.0374 0.8239 0.4933 0.026 Uiso 1 1 calc R . .
C4 C 0.0673(2) 0.6707(4) 0.54732(12) 0.0184(6) Uani 1 1 d . . .
H4 H 0.0386 0.6813 0.5768 0.022 Uiso 1 1 calc R . .
C5 C 0.15398(19) 0.5701(4) 0.55301(11) 0.0145(6) Uani 1 1 d . . .
C6 C 0.2113(2) 0.4849(4) 0.60434(11) 0.0146(6) Uani 1 1 d . . .
C7 C 0.1858(2) 0.4822(4) 0.65284(11) 0.0148(6) Uani 1 1 d . . .
H7 H 0.123 0.5276 0.6546 0.018 Uiso 1 1 calc R . .
C8 C 0.2535(2) 0.4118(4) 0.69920(11) 0.0150(5) Uani 1 1 d . . .
C9 C 0.3451(2) 0.3446(4) 0.69499(11) 0.0142(6) Uani 1 1 d . . .
H9 H 0.3931 0.3005 0.7263 0.017 Uiso 1 1 calc R . .
C10 C 0.3652(2) 0.3428(4) 0.64523(11) 0.0138(5) Uani 1 1 d . . .
C11 C 0.4533(2) 0.2634(4) 0.63221(11) 0.0138(5) Uani 1 1 d . . .
C12 C 0.5354(2) 0.1943(4) 0.67037(12) 0.0199(6) Uani 1 1 d . . .
H12 H 0.5387 0.2 0.7079 0.024 Uiso 1 1 calc R . .
C13 C 0.6131(2) 0.1166(4) 0.65345(12) 0.0238(7) Uani 1 1 d . . .
H13 H 0.6702 0.0698 0.6792 0.029 Uiso 1 1 calc R . .
C14 C 0.6060(2) 0.1086(4) 0.59889(12) 0.0216(6) Uani 1 1 d . . .
H14 H 0.6578 0.0542 0.5865 0.026 Uiso 1 1 calc R . .
C15 C 0.5228(2) 0.1802(4) 0.56212(12) 0.0181(6) Uani 1 1 d . . .
H15 H 0.5183 0.1739 0.5245 0.022 Uiso 1 1 calc R . .
C16 C 0.2293(2) 0.4061(4) 0.75186(11) 0.0164(6) Uani 1 1 d . . .
C17 C 0.1339(2) 0.3574(4) 0.75463(13) 0.0206(6) Uani 1 1 d . . .
H17 H 0.0834 0.3312 0.7224 0.025 Uiso 1 1 calc R . .
C18 C 0.1135(2) 0.3477(4) 0.80448(13) 0.0242(7) Uani 1 1 d . . .
H18 H 0.0498 0.3093 0.8065 0.029 Uiso 1 1 calc R . .
C19 C 0.1851(2) 0.3935(4) 0.85119(13) 0.0253(7) Uani 1 1 d . . .
H19 H 0.1698 0.3903 0.8851 0.03 Uiso 1 1 calc R . .
C20 C 0.2795(2) 0.4443(4) 0.84893(12) 0.0228(7) Uani 1 1 d . . .
H20 H 0.3284 0.4771 0.8812 0.027 Uiso 1 1 calc R . .
C21 C 0.3021(2) 0.4472(4) 0.79956(11) 0.0176(6) Uani 1 1 d . . .
H21 H 0.3673 0.4772 0.7981 0.021 Uiso 1 1 calc R . .
Cl1 Cl 0.23535(5) 0.11411(10) 0.51642(3) 0.01901(14) Uani 1 1 d . . .
Cl2 Cl 0.41744(5) 0.67722(10) 0.55286(3) 0.01882(15) Uani 1 1 d . . .
F1 F 0.04754(15) 0.0182(3) 0.28995(8) 0.0416(5) Uani 1 1 d . . .
F2 F 0.01422(15) 0.3162(3) 0.30875(8) 0.0364(5) Uani 1 1 d . . .
F3 F 0.14104(16) 0.3096(3) 0.38512(8) 0.0478(6) Uani 1 1 d . . .
F4 F 0.17380(16) 0.0071(4) 0.36638(9) 0.0567(7) Uani 1 1 d . . .
F5 F 0.02171(14) 0.0888(3) 0.37076(7) 0.0344(5) Uani 1 1 d . . .
F6 F 0.16855(16) 0.2361(5) 0.30439(9) 0.0688(8) Uani 1 1 d . . .
N1 N 0.34366(17) 0.3834(3) 0.46347(9) 0.0189(5) Uani 1 1 d . . .
N2 N 0.19541(16) 0.5516(3) 0.51063(9) 0.0152(5) Uani 1 1 d . . .
N3 N 0.29814(16) 0.4120(3) 0.60153(9) 0.0128(5) Uani 1 1 d . . .
N4 N 0.44816(16) 0.2585(3) 0.57824(9) 0.0140(5) Uani 1 1 d . . .
O1 O 0.34942(16) 0.3763(4) 0.42000(8) 0.0326(6) Uani 1 1 d . . .
P1 P 0.09606(6) 0.16246(13) 0.33755(3) 0.0275(2) Uani 1 1 d . . .
Ru1 Ru 0.326073(16) 0.39716(3) 0.528756(9) 0.01314(7) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.341(4) . ?
C1 C2 1.378(4) . ?
C1 H1 0.95 . ?
C2 C3 1.382(4) . ?
C2 H2 0.95 . ?
C3 C4 1.387(4) . ?
C3 H3 0.95 . ?
C4 C5 1.385(4) . ?
C4 H4 0.95 . ?
C5 N2 1.369(3) . ?
C5 C6 1.475(4) . ?
C6 N3 1.343(3) . ?
C6 C7 1.383(4) . ?
C7 C8 1.399(4) . ?
C7 H7 0.95 . ?
C8 C9 1.402(4) . ?
C8 C16 1.477(4) . ?
C9 C10 1.378(4) . ?
C9 H9 0.95 . ?
C10 N3 1.347(3) . ?
C10 C11 1.477(4) . ?
C11 N4 1.365(3) . ?
C11 C12 1.384(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.95 . ?
C13 C14 1.375(4) . ?
C13 H13 0.95 . ?
C14 C15 1.385(4) . ?
C14 H14 0.95 . ?
C15 N4 1.345(3) . ?
C15 H15 0.95 . ?
C16 C21 1.396(4) . ?
C16 C17 1.403(4) . ?
C17 C18 1.383(4) . ?
C17 H17 0.95 . ?
C18 C19 1.378(5) . ?
C18 H18 0.95 . ?
C19 C20 1.388(5) . ?
C19 H19 0.95 . ?
C20 C21 1.385(4) . ?
C20 H20 0.95 . ?
C21 H21 0.95 . ?
Cl1 Ru1 2.3598(12) . ?
Cl2 Ru1 2.3618(12) . ?
F1 P1 1.600(2) . ?
F2 P1 1.614(2) . ?
F3 P1 1.603(2) . ?
F4 P1 1.589(2) . ?
F5 P1 1.601(2) . ?
F6 P1 1.580(2) . ?
N1 O1 1.139(3) . ?
N1 Ru1 1.758(2) . ?
N2 Ru1 2.080(2) . ?
N3 Ru1 2.008(2) . ?
N4 Ru1 2.085(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
N2 C1 C2 122.0(3) . . ?
N2 C1 H1 119 . . ?
C2 C1 H1 119 . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N2 C5 C4 120.9(3) . . ?
N2 C5 C6 115.0(2) . . ?
C4 C5 C6 124.0(3) . . ?
N3 C6 C7 120.0(3) . . ?
N3 C6 C5 113.3(2) . . ?
C7 C6 C5 126.6(2) . . ?
C6 C7 C8 119.1(2) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 118.9(2) . . ?
C7 C8 C16 121.0(2) . . ?
C9 C8 C16 120.1(3) . . ?
C10 C9 C8 119.6(3) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N3 C10 C9 119.7(2) . . ?
N3 C10 C11 113.1(2) . . ?
C9 C10 C11 127.2(2) . . ?
N4 C11 C12 120.9(2) . . ?
N4 C11 C10 114.8(2) . . ?
C12 C11 C10 124.3(2) . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 119.0(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N4 C15 C14 121.8(3) . . ?
N4 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C21 C16 C17 119.3(3) . . ?
C21 C16 C8 120.1(2) . . ?
C17 C16 C8 120.6(3) . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.3(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C21 C20 C19 119.8(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C16 120.2(3) . . ?
C20 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?
O1 N1 Ru1 176.1(2) . . ?
C1 N2 C5 119.1(2) . . ?
C1 N2 Ru1 126.59(19) . . ?
C5 N2 Ru1 114.22(18) . . ?
C6 N3 C10 122.5(2) . . ?
C6 N3 Ru1 118.44(18) . . ?
C10 N3 Ru1 119.04(18) . . ?
C15 N4 C11 119.2(2) . . ?
C15 N4 Ru1 126.10(19) . . ?
C11 N4 Ru1 114.50(17) . . ?
F6 P1 F4 91.21(15) . . ?
F6 P1 F1 90.39(14) . . ?
F4 P1 F1 90.27(13) . . ?
F6 P1 F5 179.44(14) . . ?
F4 P1 F5 89.32(13) . . ?
F1 P1 F5 89.45(12) . . ?
F6 P1 F3 90.75(14) . . ?
F4 P1 F3 91.25(13) . . ?
F1 P1 F3 178.09(12) . . ?
F5 P1 F3 89.40(12) . . ?
F6 P1 F2 90.56(14) . . ?
F4 P1 F2 178.10(14) . . ?
F1 P1 F2 89.05(11) . . ?
F5 P1 F2 88.90(11) . . ?
F3 P1 F2 89.39(12) . . ?
N1 Ru1 N3 176.94(10) . . ?
N1 Ru1 N2 99.09(10) . . ?
N3 Ru1 N2 78.41(9) . . ?
N1 Ru1 N4 104.45(10) . . ?
N3 Ru1 N4 78.10(9) . . ?
N2 Ru1 N4 156.41(9) . . ?
N1 Ru1 Cl1 91.93(8) . . ?
N3 Ru1 Cl1 86.35(7) . . ?
N2 Ru1 Cl1 90.66(7) . . ?
N4 Ru1 Cl1 90.07(7) . . ?
N1 Ru1 Cl2 95.20(8) . . ?
N3 Ru1 Cl2 86.59(7) . . ?
N2 Ru1 Cl2 89.69(7) . . ?
N4 Ru1 Cl2 86.71(7) . . ?
Cl1 Ru1 Cl2 172.71(3) . . ?
####################################################################### 
# 
# 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_4t
_database_code_depnum_ccdc_archive 'CCDC 1537312'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;


#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C22 H17 Cl2 N4 O2 Ru, F6 P, C3 H6 O'
_chemical_formula_sum            'C25 H23 Cl2 F6 N4 O3 P Ru'
_chemical_formula_weight         744.41
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9624(6)
_cell_length_b                   14.2674(10)
_cell_length_c                   14.4225(11)
_cell_angle_alpha                88.839(2)
_cell_angle_beta                 80.540(2)
_cell_angle_gamma                83.493(2)
_cell_volume                     1404.08(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9961
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      30.5
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_T_max  0.7461

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_number            53554
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             8556
_reflns_number_gt                7379
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0260P)²+1.2454P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8556
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.089

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7202(3) 0.54022(12) 0.44441(13) 0.0144(3) Uani 1 1 d . . .
H1 H 0.6966 0.5228 0.3844 0.017 Uiso 1 1 calc R . .
C2 C 0.7492(3) 0.47029(13) 0.51072(14) 0.0161(4) Uani 1 1 d . . .
H2 H 0.745 0.4059 0.4963 0.019 Uiso 1 1 calc R . .
C3 C 0.7840(3) 0.49551(13) 0.59774(14) 0.0167(4) Uani 1 1 d . . .
H3 H 0.8021 0.4488 0.6443 0.02 Uiso 1 1 calc R . .
C4 C 0.7924(3) 0.58981(13) 0.61653(13) 0.0155(3) Uani 1 1 d . . .
H4 H 0.818 0.6082 0.6759 0.019 Uiso 1 1 calc R . .
C5 C 0.7634(3) 0.65658(12) 0.54815(13) 0.0129(3) Uani 1 1 d . . .
C6 C 0.7723(3) 0.75810(12) 0.56018(13) 0.0122(3) Uani 1 1 d . . .
C7 C 0.7909(3) 0.80227(13) 0.64219(13) 0.0135(3) Uani 1 1 d . . .
H7 H 0.81 0.7659 0.6965 0.016 Uiso 1 1 calc R . .
C8 C 0.7813(3) 0.90135(12) 0.64500(12) 0.0117(3) Uani 1 1 d . . .
C9 C 0.7643(3) 0.95157(12) 0.56102(12) 0.0120(3) Uani 1 1 d . . .
H9 H 0.7623 1.0183 0.5597 0.014 Uiso 1 1 calc R . .
C10 C 0.7506(2) 0.90354(12) 0.48058(12) 0.0108(3) Uani 1 1 d . . .
C11 C 0.7253(3) 0.94497(12) 0.38794(12) 0.0108(3) Uani 1 1 d . . .
C12 C 0.7369(3) 1.03893(12) 0.36513(13) 0.0130(3) Uani 1 1 d . . .
H12 H 0.7525 1.0826 0.4115 0.016 Uiso 1 1 calc R . .
C13 C 0.7255(3) 1.06888(13) 0.27388(13) 0.0157(3) Uani 1 1 d . . .
H13 H 0.7322 1.1333 0.2572 0.019 Uiso 1 1 calc R . .
C14 C 0.7044(3) 1.00388(13) 0.20762(13) 0.0151(3) Uani 1 1 d . . .
H14 H 0.7006 1.0228 0.1443 0.018 Uiso 1 1 calc R . .
C15 C 0.6889(3) 0.91077(13) 0.23435(13) 0.0141(3) Uani 1 1 d . . .
H15 H 0.6725 0.8664 0.1888 0.017 Uiso 1 1 calc R . .
C16 C 0.7811(3) 0.94983(12) 0.73421(12) 0.0124(3) Uani 1 1 d . . .
C17 C 0.7534(3) 0.90122(13) 0.82040(13) 0.0169(4) Uani 1 1 d . . .
H17 H 0.7384 0.8359 0.8206 0.02 Uiso 1 1 calc R . .
C18 C 0.7477(3) 0.94635(14) 0.90434(13) 0.0196(4) Uani 1 1 d . . .
H18 H 0.7278 0.9122 0.9617 0.024 Uiso 1 1 calc R . .
C19 C 0.7712(3) 1.04212(14) 0.90537(13) 0.0162(4) Uani 1 1 d . . .
C20 C 0.7977(3) 1.09226(13) 0.82116(13) 0.0146(3) Uani 1 1 d . . .
H20 H 0.8128 1.1576 0.8213 0.018 Uiso 1 1 calc R . .
C21 C 0.8020(3) 1.04612(13) 0.73731(12) 0.0132(3) Uani 1 1 d . . .
H21 H 0.8196 1.0808 0.6802 0.016 Uiso 1 1 calc R . .
C22 C 0.7960(4) 1.17785(15) 0.99510(15) 0.0278(5) Uani 1 1 d . . .
H22A H 0.9238 1.1879 0.9586 0.042 Uiso 1 1 calc R . .
H22B H 0.792 1.1959 1.0607 0.042 Uiso 1 1 calc R . .
H22C H 0.6923 1.2165 0.9689 0.042 Uiso 1 1 calc R . .
C23 C 0.7622(4) 0.67594(16) 0.03494(16) 0.0274(5) Uani 1 1 d . . .
C24 C 0.9151(4) 0.61834(18) 0.07973(17) 0.0331(5) Uani 1 1 d . . .
H24A H 0.9438 0.6532 0.1328 0.05 Uiso 1 1 calc R . .
H24B H 1.0348 0.6054 0.0335 0.05 Uiso 1 1 calc R . .
H24C H 0.8672 0.5586 0.1023 0.05 Uiso 1 1 calc R . .
C25 C 0.6950(5) 0.6308(2) -0.0449(2) 0.0480(7) Uani 1 1 d . . .
H25A H 0.6355 0.5738 -0.0225 0.072 Uiso 1 1 calc R . .
H25B H 0.8073 0.6141 -0.0944 0.072 Uiso 1 1 calc R . .
H25C H 0.598 0.6751 -0.07 0.072 Uiso 1 1 calc R . .
F1 F 0.9021(2) 0.27584(10) 0.20743(12) 0.0400(4) Uani 1 1 d . . .
F2 F 0.7183(3) 0.34565(12) 0.33633(10) 0.0485(4) Uani 1 1 d . . .
F3 F 0.5762(2) 0.45338(10) 0.24470(12) 0.0405(4) Uani 1 1 d . . .
F4 F 0.7576(2) 0.38347(10) 0.11623(9) 0.0316(3) Uani 1 1 d . . .
F5 F 0.9051(2) 0.43197(10) 0.23218(10) 0.0339(3) Uani 1 1 d . . .
F6 F 0.5718(2) 0.29650(9) 0.22072(10) 0.0308(3) Uani 1 1 d . . .
N1 N 0.5853(2) 0.69080(11) 0.28322(11) 0.0154(3) Uani 1 1 d . . .
N2 N 0.7246(2) 0.63171(10) 0.46287(11) 0.0121(3) Uani 1 1 d . . .
N3 N 0.7549(2) 0.80883(10) 0.48190(10) 0.0118(3) Uani 1 1 d . . .
N4 N 0.6963(2) 0.88187(10) 0.32290(10) 0.0117(3) Uani 1 1 d . . .
O1 O 0.4981(2) 0.65926(11) 0.23463(11) 0.0259(3) Uani 1 1 d . . .
O2 O 0.7669(2) 1.08023(10) 0.99097(10) 0.0241(3) Uani 1 1 d . . .
O3 O 0.6956(3) 0.75507(12) 0.06182(13) 0.0357(4) Uani 1 1 d . . .
P1 P 0.73808(8) 0.36454(4) 0.22623(4) 0.01950(11) Uani 1 1 d . . .
Ru1 Ru 0.68457(2) 0.744507(10) 0.371963(10) 0.01050(4) Uani 1 1 d . . .
Cl1 Cl 1.01644(6) 0.71583(3) 0.30756(3) 0.01644(9) Uani 1 1 d . . .
Cl2 Cl 0.35868(6) 0.78331(3) 0.45160(3) 0.01450(8) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.342(2) . ?
C1 C2 1.389(3) . ?
C1 H1 0.95 . ?
C2 C3 1.379(3) . ?
C2 H2 0.95 . ?
C3 C4 1.388(3) . ?
C3 H3 0.95 . ?
C4 C5 1.380(2) . ?
C4 H4 0.95 . ?
C5 N2 1.364(2) . ?
C5 C6 1.472(2) . ?
C6 N3 1.343(2) . ?
C6 C7 1.383(2) . ?
C7 C8 1.409(2) . ?
C7 H7 0.95 . ?
C8 C9 1.410(2) . ?
C8 C16 1.473(2) . ?
C9 C10 1.381(2) . ?
C9 H9 0.95 . ?
C10 N3 1.348(2) . ?
C10 C11 1.479(2) . ?
C11 N4 1.367(2) . ?
C11 C12 1.382(2) . ?
C12 C13 1.387(3) . ?
C12 H12 0.95 . ?
C13 C14 1.381(3) . ?
C13 H13 0.95 . ?
C14 C15 1.387(3) . ?
C14 H14 0.95 . ?
C15 N4 1.341(2) . ?
C15 H15 0.95 . ?
C16 C21 1.400(2) . ?
C16 C17 1.407(2) . ?
C17 C18 1.376(3) . ?
C17 H17 0.95 . ?
C18 C19 1.395(3) . ?
C18 H18 0.95 . ?
C19 O2 1.354(2) . ?
C19 C20 1.394(3) . ?
C20 C21 1.383(2) . ?
C20 H20 0.95 . ?
C21 H21 0.95 . ?
C22 O2 1.434(3) . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 O3 1.217(3) . ?
C23 C24 1.494(3) . ?
C23 C25 1.495(3) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
F1 P1 1.6010(15) . ?
F2 P1 1.5912(15) . ?
F3 P1 1.5935(15) . ?
F4 P1 1.5902(14) . ?
F5 P1 1.6044(14) . ?
F6 P1 1.6053(14) . ?
N1 O1 1.130(2) . ?
N1 Ru1 1.7757(16) . ?
N2 Ru1 2.0783(15) . ?
N3 Ru1 2.0031(15) . ?
N4 Ru1 2.0759(15) . ?
Ru1 Cl1 2.3377(5) . ?
Ru1 Cl2 2.3787(5) . ?

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 C1 C2 121.77(17) . . ?
N2 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.12(17) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.32(17) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.32(18) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N2 C5 C4 121.26(17) . . ?
N2 C5 C6 115.01(15) . . ?
C4 C5 C6 123.74(17) . . ?
N3 C6 C7 120.31(16) . . ?
N3 C6 C5 113.38(16) . . ?
C7 C6 C5 126.29(16) . . ?
C6 C7 C8 119.82(16) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 117.78(16) . . ?
C7 C8 C16 120.34(16) . . ?
C9 C8 C16 121.83(16) . . ?
C10 C9 C8 119.83(16) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
N3 C10 C9 120.27(16) . . ?
N3 C10 C11 112.75(15) . . ?
C9 C10 C11 126.96(16) . . ?
N4 C11 C12 121.05(16) . . ?
N4 C11 C10 114.73(15) . . ?
C12 C11 C10 124.17(16) . . ?
C11 C12 C13 119.35(17) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 119.19(17) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 119.36(17) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N4 C15 C14 121.60(17) . . ?
N4 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C21 C16 C17 117.32(16) . . ?
C21 C16 C8 121.78(16) . . ?
C17 C16 C8 120.87(16) . . ?
C18 C17 C16 121.38(17) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 120.13(17) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
O2 C19 C20 124.15(17) . . ?
O2 C19 C18 116.05(17) . . ?
C20 C19 C18 119.80(17) . . ?
C21 C20 C19 119.46(17) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C16 121.90(16) . . ?
C20 C21 H21 119.1 . . ?
C16 C21 H21 119.1 . . ?
O2 C22 H22A 109.5 . . ?
O2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C24 122.1(2) . . ?
O3 C23 C25 121.7(2) . . ?
C24 C23 C25 116.2(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O1 N1 Ru1 170.52(16) . . ?
C1 N2 C5 119.18(16) . . ?
C1 N2 Ru1 126.59(13) . . ?
C5 N2 Ru1 114.21(11) . . ?
C6 N3 C10 121.90(15) . . ?
C6 N3 Ru1 118.35(12) . . ?
C10 N3 Ru1 118.79(12) . . ?
C15 N4 C11 119.36(15) . . ?
C15 N4 Ru1 125.88(12) . . ?
C11 N4 Ru1 114.65(11) . . ?
C19 O2 C22 117.93(16) . . ?
F4 P1 F2 179.94(13) . . ?
F4 P1 F3 89.73(9) . . ?
F2 P1 F3 90.22(9) . . ?
F4 P1 F1 90.12(9) . . ?
F2 P1 F1 89.94(10) . . ?
F3 P1 F1 179.53(9) . . ?
F4 P1 F5 89.98(8) . . ?
F2 P1 F5 90.05(8) . . ?
F3 P1 F5 89.58(8) . . ?
F1 P1 F5 89.97(8) . . ?
F4 P1 F6 90.30(8) . . ?
F2 P1 F6 89.68(8) . . ?
F3 P1 F6 90.73(8) . . ?
F1 P1 F6 89.71(8) . . ?
F5 P1 F6 179.58(9) . . ?
N1 Ru1 N3 171.41(7) . . ?
N1 Ru1 N4 102.37(7) . . ?
N3 Ru1 N4 78.23(6) . . ?
N1 Ru1 N2 101.28(7) . . ?
N3 Ru1 N2 78.51(6) . . ?
N4 Ru1 N2 156.33(6) . . ?
N1 Ru1 Cl1 98.57(5) . . ?
N3 Ru1 Cl1 90.02(5) . . ?
N4 Ru1 Cl1 87.14(4) . . ?
N2 Ru1 Cl1 88.53(4) . . ?
N1 Ru1 Cl2 88.08(5) . . ?
N3 Ru1 Cl2 83.34(5) . . ?
N4 Ru1 Cl2 91.11(4) . . ?
N2 Ru1 Cl2 90.52(4) . . ?
Cl1 Ru1 Cl2 173.347(17) . . ?
####################################################################### 
# 
# 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_4i
_database_code_depnum_ccdc_archive 'CCDC 1537315'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;



#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C24 H20 Cl2 N4 O Ru, F6 P'
_chemical_formula_sum            'C24 H20 Cl2 F6 N4 O P Ru'
_chemical_formula_weight         697.38
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
_cell_length_a                   7.6187(8)
_cell_length_b                   25.999(3)
_cell_length_c                   13.6071(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.433(11)
_cell_angle_gamma                90
_cell_volume                     2621.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    3814
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      24.96
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'yellow green'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_T_max  0.9987

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1978
_diffrn_orient_matrix_ub_11      0.091796
_diffrn_orient_matrix_ub_12      -0.0061465
_diffrn_orient_matrix_ub_13      0.0213659
_diffrn_orient_matrix_ub_21      -0.0217069
_diffrn_orient_matrix_ub_22      -0.026598
_diffrn_orient_matrix_ub_23      -0.0039464
_diffrn_orient_matrix_ub_31      0.017408
_diffrn_orient_matrix_ub_32      -0.0005775
_diffrn_orient_matrix_ub_33      -0.0490622
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.1051
_diffrn_reflns_av_unetI/netI     0.161
_diffrn_reflns_number            26342
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.928
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_full        24.712
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_ful 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_number_total             4454
_reflns_number_gt                3133
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+21.0153P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4454
_refine_ls_number_parameters     364
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.147
_refine_ls_wR_factor_gt          0.1336
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.09
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.116

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4853(11) 0.3532(4) 0.4437(6) 0.041(2) Uani 1 d . .
H1 H 0.527731 0.326853 0.406728 0.049 Uiso 1 calc . .
C2 C 0.4951(12) 0.3463(4) 0.5457(7) 0.047(2) Uani 1 d . .
H2 H 0.545673 0.315592 0.578169 0.057 Uiso 1 calc . .
C3 C 0.4319(11) 0.3837(4) 0.6004(6) 0.046(2) Uani 1 d . .
H3 H 0.439357 0.37943 0.670551 0.055 Uiso 1 calc . .
C4 C 0.3567(10) 0.4280(4) 0.5498(6) 0.038(2) Uani 1 d . .
H4 H 0.311009 0.454405 0.585171 0.046 Uiso 1 calc . .
C5 C 0.3493(10) 0.4331(3) 0.4480(5) 0.032(2) Uani 1 d . .
C6 C 0.2695(10) 0.4787(3) 0.3886(5) 0.032(2) Uani 1 d . .
C7 C 0.1945(10) 0.5207(3) 0.4214(6) 0.034(2) Uani 1 d . .
H7 H 0.184655 0.522017 0.489642 0.041 Uiso 1 calc . .
C8 C 0.1315(10) 0.5620(3) 0.3579(6) 0.0319(19) Uani 1 d . .
C9 C 0.1477(10) 0.5581(3) 0.2566(5) 0.0303(19) Uani 1 d . .
H9 H 0.107701 0.585463 0.210642 0.036 Uiso 1 calc . .
C10 C 0.2221(10) 0.5143(3) 0.2244(5) 0.0310(19) Uani 1 d . .
C11 C 0.2457(10) 0.5031(3) 0.1216(5) 0.0305(19) Uani 1 d . .
C12 C 0.1925(10) 0.5353(4) 0.0401(6) 0.038(2) Uani 1 d . .
H12 H 0.140749 0.567758 0.048512 0.046 Uiso 1 calc . .
C13 C 0.2140(11) 0.5206(4) -0.0541(6) 0.040(2) Uani 1 d . .
H13 H 0.177079 0.542596 -0.110924 0.048 Uiso 1 calc . .
C14 C 0.2899(11) 0.4736(4) -0.0638(5) 0.039(2) Uani 1 d . .
H14 H 0.304408 0.462556 -0.127959 0.046 Uiso 1 calc . .
C15 C 0.3455(10) 0.4420(4) 0.0199(6) 0.037(2) Uani 1 d . .
H15 H 0.399386 0.40971 0.012849 0.044 Uiso 1 calc . .
C16 C 0.6262(14) 0.3227(4) 0.1921(6) 0.044(2) Uani 1 d . .
C17 C 0.7548(15) 0.2824(4) 0.1767(8) 0.064(3) Uani 1 d . .
H17A H 0.876741 0.296891 0.189607 0.096 Uiso 1 calc . .
H17B H 0.719995 0.269835 0.106984 0.096 Uiso 1 calc . .
H17C H 0.752642 0.253821 0.223391 0.096 Uiso 1 calc . .
C18 C 0.0569(10) 0.6088(3) 0.3947(6) 0.037(2) Uani 1 d . .
C19 C 0.0686(11) 0.6161(4) 0.4973(7) 0.049(3) Uani 1 d . .
H19 H 0.122051 0.589831 0.542989 0.059 Uiso 1 calc . .
C20 C 0.0064(12) 0.6596(4) 0.5357(8) 0.057(3) Uani 1 d . .
H20 H 0.014525 0.662656 0.606141 0.068 Uiso 1 calc . .
C21 C -0.0679(13) 0.6986(4) 0.4705(8) 0.056(3) Uani 1 d . .
O1A O -0.123(7) 0.7442(8) 0.500(2) 0.107(6) Uani 0.55 d A 1
C24A C -0.119(3) 0.7580(8) 0.5884(14) 0.060(4) Uani 0.55 d A 1
H24A H -0.195224 0.735032 0.617572 0.09 Uiso 0.55 calc A 1
H24B H -0.163469 0.793318 0.588082 0.09 Uiso 0.55 calc A 1
H24C H 0.005599 0.756317 0.628954 0.09 Uiso 0.55 calc A 1
C24B C -0.155(3) 0.7821(9) 0.4755(18) 0.060(4) Uani 0.45 d A 2
H24D H -0.03919 0.791545 0.46135 0.09 Uiso 0.45 calc A 2
H24E H -0.184293 0.806151 0.524992 0.09 Uiso 0.45 calc A 2
H24F H -0.249887 0.783684 0.412955 0.09 Uiso 0.45 calc A 2
O1B O -0.146(9) 0.7375(11) 0.510(3) 0.107(6) Uani 0.45 d A 2
C22 C -0.0801(15) 0.6935(4) 0.3684(8) 0.063(3) Uani 1 d . .
H22 H -0.128931 0.720582 0.323604 0.076 Uiso 1 calc . .
C23 C -0.0204(13) 0.6481(4) 0.3306(8) 0.054(3) Uani 1 d . .
H23 H -0.033461 0.644289 0.259861 0.065 Uiso 1 calc . .
N2 N 0.4176(8) 0.3961(3) 0.3966(4) 0.0335(17) Uani 1 d . .
N3 N 0.2790(8) 0.4760(3) 0.2896(4) 0.0315(16) Uani 1 d . .
N4 N 0.3238(8) 0.4569(3) 0.1111(4) 0.0326(16) Uani 1 d . .
N1 N 0.5349(11) 0.3544(3) 0.2065(5) 0.0431(19) Uani 1 d . .
F1 F 0.4671(10) 0.6215(3) 0.1491(4) 0.090(2) Uani 1 d . .
F2 F 0.2776(13) 0.6728(3) 0.1938(8) 0.152(4) Uani 1 d . .
F3 F 0.5427(13) 0.7026(4) 0.2040(6) 0.149(4) Uani 1 d . .
F4 F 0.2493(14) 0.6555(3) 0.0319(7) 0.162(5) Uani 1 d . .
F5 F 0.5123(13) 0.6833(4) 0.0396(7) 0.161(4) Uani 1 d . .
F6 F 0.3190(10) 0.7340(2) 0.0870(5) 0.087(2) Uani 1 d . .
P1 P 0.3962(4) 0.67882(12) 0.11802(19) 0.0550(7) Uani 1 d . .
CL1 Cl 0.1213(3) 0.37387(10) 0.20206(16) 0.0495(6) Uani 1 d . .
CL2 Cl 0.6721(3) 0.46049(9) 0.28948(13) 0.0366(5) Uani 1 d . .
RU1 Ru 0.39572(9) 0.41618(3) 0.24611(5) 0.0347(2) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.329(10) . ?
C1 C2 1.384(11) . ?
C2 C3 1.377(13) . ?
C3 C4 1.394(12) . ?
C4 C5 1.380(10) . ?
C5 N2 1.363(10) . ?
C5 C6 1.482(11) . ?
C6 C7 1.355(11) . ?
C6 N3 1.368(9) . ?
C7 C8 1.392(11) . ?
C8 C9 1.416(10) . ?
C8 C18 1.478(11) . ?
C9 C10 1.388(11) . ?
C10 N3 1.336(10) . ?
C10 C11 1.480(10) . ?
C11 N4 1.361(10) . ?
C11 C12 1.374(11) . ?
C12 C13 1.384(11) . ?
C13 C14 1.371(12) . ?
C14 C15 1.387(11) . ?
C15 N4 1.346(9) . ?
C16 N1 1.124(11) . ?
C16 C17 1.482(13) . ?
C18 C23 1.382(12) . ?
C18 C19 1.391(11) . ?
C19 C20 1.373(13) . ?
C20 C21 1.380(14) . ?
C21 O1A 1.348(15) . ?
C21 O1B 1.349(10) . ?
C21 C22 1.377(14) . ?
O1Aa C24A 1.250(10) . ?
C24Bb O1B 1.250(10) . ?
C22 C23 1.405(13) . ?
N2 RU1 2.082(6) . ?
N3 RU1 1.951(7) . ?
N4 RU1 2.080(6) . ?
N1 RU1 2.064(8) . ?
F1 P1 1.608(7) . ?
F2 P1 1.529(7) . ?
F3 P1 1.546(8) . ?
F4 P1 1.544(8) . ?
F5 P1 1.540(8) . ?
F6 P1 1.572(7) . ?
CL1 RU1 2.314(2) . ?
CL2 RU1 2.352(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
N2 C1 C2 121.1(8) . . ?
C3 C2 C1 120.4(9) . . ?
C2 C3 C4 118.1(8) . . ?
C5 C4 C3 119.5(8) . . ?
N2 C5 C4 121.0(8) . . ?
N2 C5 C6 116.2(6) . . ?
C4 C5 C6 122.7(8) . . ?
C7 C6 N3 119.1(8) . . ?
C7 C6 C5 128.0(7) . . ?
N3 C6 C5 112.8(7) . . ?
C6 C7 C8 122.0(7) . . ?
C7 C8 C9 116.9(7) . . ?
C7 C8 C18 121.9(7) . . ?
C9 C8 C18 121.1(8) . . ?
C10 C9 C8 120.1(7) . . ?
N3 C10 C9 119.7(7) . . ?
N3 C10 C11 112.9(7) . . ?
C9 C10 C11 127.5(7) . . ?
N4 C11 C12 120.5(7) . . ?
N4 C11 C10 115.1(7) . . ?
C12 C11 C10 124.4(8) . . ?
C11 C12 C13 120.2(9) . . ?
C14 C13 C12 118.5(8) . . ?
C13 C14 C15 120.2(8) . . ?
N4 C15 C14 120.5(8) . . ?
N1 C16 C17 176.9(11) . . ?
C23 C18 C19 116.7(9) . . ?
C23 C18 C8 122.4(8) . . ?
C19 C18 C8 120.9(8) . . ?
C20 C19 C18 123.2(10) . . ?
C19 C20 C21 119.2(9) . . ?
O1Aa C21 C22 115.6(14) . . ?
O1Bb C21 C22 123.1(18) . . ?
O1Aa C21 C20 124.5(14) . . ?
O1Bb C21 C20 116.5(16) . . ?
C22 C21 C20 119.8(9) . . ?
C24Aa O1Aa C21 127(2) . . ?
C24Bb O1Bb C21 122(3) . . ?
C21 C22 C23 120.0(10) . . ?
C18 C23 C22 121.1(9) . . ?
C1 N2 C5 119.8(7) . . ?
C1 N2 RU1 128.2(6) . . ?
C5 N2 RU1 112.0(5) . . ?
C10 N3 C6 122.2(7) . . ?
C10 N3 RU1 119.5(5) . . ?
C6 N3 RU1 118.1(6) . . ?
C15 N4 C11 120.0(7) . . ?
C15 N4 RU1 127.2(6) . . ?
C11 N4 RU1 112.8(5) . . ?
C16 N1 RU1 172.6(8) . . ?
F2 P1 F5 178.1(7) . . ?
F2 P1 F4 92.0(6) . . ?
F5 P1 F4 86.3(6) . . ?
F2 P1 F3 88.1(6) . . ?
F5 P1 F3 93.7(6) . . ?
F4 P1 F3 179.5(5) . . ?
F2 P1 F6 91.8(4) . . ?
F5 P1 F6 89.1(5) . . ?
F4 P1 F6 89.7(4) . . ?
F3 P1 F6 89.8(5) . . ?
F2 P1 F1 86.8(4) . . ?
F5 P1 F1 92.3(5) . . ?
F4 P1 F1 88.6(4) . . ?
F3 P1 F1 91.9(5) . . ?
F6 P1 F1 177.7(4) . . ?
N3 RU1 N1 176.2(3) . . ?
N3 RU1 N4 79.4(3) . . ?
N1 RU1 N4 102.2(3) . . ?
N3 RU1 N2 80.8(3) . . ?
N1 RU1 N2 97.7(3) . . ?
N4 RU1 N2 160.1(3) . . ?
N3 RU1 CL1 90.55(19) . . ?
N1 RU1 CL1 92.9(2) . . ?
N4 RU1 CL1 88.64(18) . . ?
N2 RU1 CL1 89.82(18) . . ?
N3 RU1 CL2 88.74(19) . . ?
N1 RU1 CL2 87.8(2) . . ?
N4 RU1 CL2 90.53(18) . . ?
N2 RU1 CL2 90.77(18) . . ?
CL1 RU1 CL2 178.99(9) . . ?


#===END



####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1537311'
_audit_update_record             
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;


#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H14 Br Cl2 N4 O Ru, F6 P'
_chemical_formula_sum            'C21 H14 Br Cl2 F6 N4 O P Ru'
_chemical_formula_weight         735.20
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_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                   10.8897(9)
_cell_length_b                   17.2969(13)
_cell_length_c                   13.3346(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.353(3)
_cell_angle_gamma                90
_cell_volume                     2422.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9902
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      26.24
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_T_max  0.7461

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_number            50815
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_full        26.73
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             5140
_reflns_number_gt                4154
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0348P)²+5.2349P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5140
_refine_ls_number_parameters     390
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.636
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.108

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5000(4) 0.4240(2) 0.8088(3) 0.0244(8) Uani 1 1 d . . .
H1 H 0.5421 0.4337 0.8797 0.029 Uiso 1 1 calc R . .
C2 C 0.4789(4) 0.3488(2) 0.7747(3) 0.0262(9) Uani 1 1 d . . .
H2 H 0.505 0.307 0.8218 0.031 Uiso 1 1 calc R . .
C3 C 0.4198(4) 0.3348(2) 0.6717(3) 0.0252(8) Uani 1 1 d . . .
H3 H 0.4048 0.2831 0.6475 0.03 Uiso 1 1 calc R . .
C4 C 0.3818(4) 0.3959(2) 0.6031(3) 0.0206(8) Uani 1 1 d . . .
H4 H 0.3416 0.3867 0.5317 0.025 Uiso 1 1 calc R . .
C5 C 0.4038(3) 0.4707(2) 0.6412(3) 0.0183(7) Uani 1 1 d . . .
C6 C 0.3634(3) 0.54069(19) 0.5776(3) 0.0165(7) Uani 1 1 d . . .
C7 C 0.3214(3) 0.54455(19) 0.4705(3) 0.0171(7) Uani 1 1 d . . .
H7 H 0.3153 0.4989 0.4299 0.02 Uiso 1 1 calc R . .
C8 C 0.2876(3) 0.61664(19) 0.4216(3) 0.0165(7) Uani 1 1 d . . .
C9 C 0.3008(3) 0.6828(2) 0.4843(3) 0.0169(7) Uani 1 1 d . . .
H9 H 0.2788 0.7321 0.4533 0.02 Uiso 1 1 calc R . .
C10 C 0.3460(3) 0.67633(19) 0.5914(3) 0.0160(7) Uani 1 1 d . . .
C11 C 0.3710(3) 0.7397(2) 0.6679(3) 0.0176(7) Uani 1 1 d . . .
C12 C 0.3389(4) 0.8154(2) 0.6427(3) 0.0221(8) Uani 1 1 d . . .
H12 H 0.2983 0.8295 0.5729 0.026 Uiso 1 1 calc R . .
C13 C 0.3664(4) 0.8713(2) 0.7207(3) 0.0256(8) Uani 1 1 d . . .
H13 H 0.344 0.9238 0.7047 0.031 Uiso 1 1 calc R . .
C14 C 0.4265(4) 0.8498(2) 0.8210(3) 0.0257(8) Uani 1 1 d . . .
H14 H 0.446 0.8872 0.8751 0.031 Uiso 1 1 calc R . .
C15 C 0.4580(4) 0.7730(2) 0.8421(3) 0.0225(8) Uani 1 1 d . . .
H15 H 0.4998 0.7581 0.9113 0.027 Uiso 1 1 calc R . .
C16 C 0.2354(4) 0.6215(2) 0.3079(3) 0.0185(7) Uani 1 1 d . . .
C17 C 0.1799(4) 0.5568(2) 0.2508(3) 0.0214(8) Uani 1 1 d . . .
H17 H 0.1816 0.5085 0.285 0.026 Uiso 1 1 calc R . .
C18 C 0.1226(4) 0.5618(2) 0.1449(3) 0.0262(9) Uani 1 1 d . . .
H18 H 0.0861 0.5175 0.1064 0.031 Uiso 1 1 calc R . .
C19 C 0.1196(4) 0.6325(2) 0.0967(3) 0.0235(8) Uani 1 1 d . . .
C20 C 0.1777(4) 0.6973(2) 0.1496(3) 0.0245(8) Uani 1 1 d . . .
H20 H 0.1782 0.7449 0.1142 0.029 Uiso 1 1 calc R . .
C21 C 0.2348(4) 0.6913(2) 0.2550(3) 0.0218(8) Uani 1 1 d . . .
H21 H 0.2745 0.7355 0.2922 0.026 Uiso 1 1 calc R . .
Br1 Br 0.02724(4) 0.64194(2) -0.04571(3) 0.03048(12) Uani 1 1 d . . .
Cl1 Cl 0.59370(10) 0.59607(6) 0.95837(7) 0.0326(2) Uani 1 1 d . . .
Cl2 Cl 0.64419(9) 0.61435(5) 0.72711(8) 0.0252(2) Uani 1 1 d . . .
P1 P 1.00798(9) 0.62209(6) 0.63749(7) 0.0218(2) Uani 1 1 d U . .
F1 F 1.0820(9) 0.5958(5) 0.5588(7) 0.0354(17) Uani 0.670(17) 1 d PU A 1
F2 F 1.0538(8) 0.5501(4) 0.7104(6) 0.0458(18) Uani 0.670(17) 1 d PU A 1
F3 F 0.9310(6) 0.6545(6) 0.7199(4) 0.0364(15) Uani 0.670(17) 1 d PU A 1
F4 F 0.9585(10) 0.6987(6) 0.5680(7) 0.0345(18) Uani 0.670(17) 1 d PU A 1
F5 F 0.8828(10) 0.5791(6) 0.5756(9) 0.0316(18) Uani 0.670(17) 1 d PU A 1
F6 F 1.130(2) 0.6703(16) 0.7083(14) 0.028(2) Uani 0.670(17) 1 d PU A 1
F1' F 1.081(2) 0.6213(10) 0.5422(14) 0.034(3) Uani 0.330(17) 1 d PU A 2
F2' F 1.0959(16) 0.5448(8) 0.6800(12) 0.042(3) Uani 0.330(17) 1 d PU A 2
F3' F 0.9441(14) 0.6174(11) 0.7232(10) 0.042(3) Uani 0.330(17) 1 d PU A 2
F4' F 0.9288(19) 0.6916(14) 0.5847(16) 0.038(3) Uani 0.330(17) 1 d PU A 2
F5' F 0.905(2) 0.5601(11) 0.5653(19) 0.028(3) Uani 0.330(17) 1 d PU A 2
F6' F 1.120(5) 0.675(3) 0.692(3) 0.025(3) Uani 0.330(17) 1 d PU A 2
N1 N 0.3327(3) 0.58419(18) 0.8389(2) 0.0236(7) Uani 1 1 d . . .
N2 N 0.4624(3) 0.48397(17) 0.7437(2) 0.0197(6) Uani 1 1 d . . .
N3 N 0.3723(3) 0.60581(16) 0.6340(2) 0.0153(6) Uani 1 1 d . . .
N4 N 0.4312(3) 0.71896(17) 0.7675(2) 0.0186(6) Uani 1 1 d . . .
O1 O 0.2639(3) 0.5688(2) 0.8862(2) 0.0374(7) Uani 1 1 d . . .
Ru1 Ru 0.46111(3) 0.599943(16) 0.78413(2) 0.01724(9) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.345(5) . ?
C1 C2 1.377(5) . ?
C1 H1 0.95 . ?
C2 C3 1.375(6) . ?
C2 H2 0.95 . ?
C3 C4 1.388(5) . ?
C3 H3 0.95 . ?
C4 C5 1.387(5) . ?
C4 H4 0.95 . ?
C5 N2 1.367(4) . ?
C5 C6 1.477(5) . ?
C6 N3 1.343(4) . ?
C6 C7 1.382(5) . ?
C7 C8 1.410(5) . ?
C7 H7 0.95 . ?
C8 C9 1.402(5) . ?
C8 C16 1.474(5) . ?
C9 C10 1.387(5) . ?
C9 H9 0.95 . ?
C10 N3 1.344(4) . ?
C10 C11 1.472(5) . ?
C11 N4 1.364(4) . ?
C11 C12 1.374(5) . ?
C12 C13 1.393(5) . ?
C12 H12 0.95 . ?
C13 C14 1.376(5) . ?
C13 H13 0.95 . ?
C14 C15 1.383(5) . ?
C14 H14 0.95 . ?
C15 N4 1.339(4) . ?
C15 H15 0.95 . ?
C16 C21 1.397(5) . ?
C16 C17 1.399(5) . ?
C17 C18 1.387(5) . ?
C17 H17 0.95 . ?
C18 C19 1.378(5) . ?
C18 H18 0.95 . ?
C19 C20 1.384(5) . ?
C19 Br1 1.906(4) . ?
C20 C21 1.382(5) . ?
C20 H20 0.95 . ?
C21 H21 0.95 . ?
Cl1 Ru1 2.3898(10) . ?
Cl2 Ru1 2.3276(10) . ?
P1 F3' 1.489(14) . ?
P1 F4' 1.54(2) . ?
P1 F1 1.550(9) . ?
P1 F6' 1.55(5) . ?
P1 F2 1.577(7) . ?
P1 F5 1.580(11) . ?
P1 F4 1.625(10) . ?
P1 F6 1.64(2) . ?
P1 F3 1.647(6) . ?
P1 F2' 1.654(14) . ?
P1 F5' 1.66(2) . ?
P1 F1' 1.67(2) . ?
N1 O1 1.132(4) . ?
N1 Ru1 1.761(3) . ?
N2 Ru1 2.078(3) . ?
N3 Ru1 1.982(3) . ?
N4 Ru1 2.087(3) . ?

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 C1 C2 121.3(4) . . ?
N2 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N2 C5 C4 120.9(3) . . ?
N2 C5 C6 115.2(3) . . ?
C4 C5 C6 123.9(3) . . ?
N3 C6 C7 119.6(3) . . ?
N3 C6 C5 113.6(3) . . ?
C7 C6 C5 126.9(3) . . ?
C6 C7 C8 119.7(3) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 C16 121.1(3) . . ?
C7 C8 C16 120.5(3) . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120 . . ?
C8 C9 H9 120 . . ?
N3 C10 C9 119.1(3) . . ?
N3 C10 C11 113.8(3) . . ?
C9 C10 C11 127.1(3) . . ?
N4 C11 C12 120.9(3) . . ?
N4 C11 C10 115.6(3) . . ?
C12 C11 C10 123.5(3) . . ?
C11 C12 C13 119.3(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 119.4(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
N4 C15 C14 121.7(3) . . ?
N4 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C21 C16 C17 118.2(3) . . ?
C21 C16 C8 121.2(3) . . ?
C17 C16 C8 120.6(3) . . ?
C18 C17 C16 121.1(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C19 C18 C17 118.6(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C20 122.0(3) . . ?
C18 C19 Br1 118.8(3) . . ?
C20 C19 Br1 119.2(3) . . ?
C21 C20 C19 118.7(3) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C16 121.2(3) . . ?
C20 C21 H21 119.4 . . ?
C16 C21 H21 119.4 . . ?
F3' P1 F4' 94.3(8) . . ?
F3' P1 F1 159.3(6) . . ?
F4' P1 F1 104.4(7) . . ?
F3' P1 F6' 98(2) . . ?
F4' P1 F6' 91.6(19) . . ?
F1 P1 F6' 90(2) . . ?
F3' P1 F2 67.7(6) . . ?
F4' P1 F2 161.3(6) . . ?
F1 P1 F2 92.8(3) . . ?
F6' P1 F2 95.6(17) . . ?
F3' P1 F5 82.1(6) . . ?
F4' P1 F5 80.0(9) . . ?
F1 P1 F5 92.3(5) . . ?
F6' P1 F5 171.6(18) . . ?
F2 P1 F5 92.2(5) . . ?
F3' P1 F4 109.3(7) . . ?
F1 P1 F4 90.4(4) . . ?
F6' P1 F4 83.3(17) . . ?
F2 P1 F4 176.7(4) . . ?
F5 P1 F4 88.6(5) . . ?
F3' P1 F6 93.4(10) . . ?
F4' P1 F6 97.9(12) . . ?
F1 P1 F6 92.9(10) . . ?
F2 P1 F6 88.3(8) . . ?
F5 P1 F6 174.8(11) . . ?
F4 P1 F6 90.6(9) . . ?
F4' P1 F3 73.5(7) . . ?
F1 P1 F3 177.1(3) . . ?
F6' P1 F3 88(2) . . ?
F2 P1 F3 89.5(3) . . ?
F5 P1 F3 89.3(4) . . ?
F4 P1 F3 87.2(4) . . ?
F6 P1 F3 85.5(10) . . ?
F3' P1 F2' 92.2(6) . . ?
F4' P1 F2' 172.9(9) . . ?
F1 P1 F2' 68.8(5) . . ?
F6' P1 F2' 90.3(19) . . ?
F5 P1 F2' 98.1(6) . . ?
F4 P1 F2' 158.2(6) . . ?
F6 P1 F2' 84.5(10) . . ?
F3 P1 F2' 113.4(5) . . ?
F3' P1 F5' 91.6(9) . . ?
F4' P1 F5' 91.6(11) . . ?
F1 P1 F5' 79.2(8) . . ?
F6' P1 F5' 169(2) . . ?
F2 P1 F5' 84.5(8) . . ?
F4 P1 F5' 97.1(8) . . ?
F6 P1 F5' 168.9(11) . . ?
F3 P1 F5' 102.7(7) . . ?
F2' P1 F5' 85.4(8) . . ?
F3' P1 F1' 176.4(7) . . ?
F4' P1 F1' 88.8(8) . . ?
F6' P1 F1' 83(2) . . ?
F2 P1 F1' 109.0(6) . . ?
F5 P1 F1' 96.7(8) . . ?
F4 P1 F1' 74.0(6) . . ?
F6 P1 F1' 88.0(12) . . ?
F3 P1 F1' 160.1(5) . . ?
F2' P1 F1' 84.6(7) . . ?
F5' P1 F1' 86.5(10) . . ?
O1 N1 Ru1 169.4(3) . . ?
C1 N2 C5 119.8(3) . . ?
C1 N2 Ru1 126.8(3) . . ?
C5 N2 Ru1 112.9(2) . . ?
C6 N3 C10 123.3(3) . . ?
C6 N3 Ru1 117.8(2) . . ?
C10 N3 Ru1 117.8(2) . . ?
C15 N4 C11 119.6(3) . . ?
C15 N4 Ru1 127.7(2) . . ?
C11 N4 Ru1 112.6(2) . . ?
N1 Ru1 N3 101.42(13) . . ?
N1 Ru1 N2 91.06(13) . . ?
N3 Ru1 N2 79.77(11) . . ?
N1 Ru1 N4 94.47(13) . . ?
N3 Ru1 N4 79.71(11) . . ?
N2 Ru1 N4 159.42(11) . . ?
N1 Ru1 Cl2 173.99(10) . . ?
N3 Ru1 Cl2 84.00(9) . . ?
N2 Ru1 Cl2 87.34(9) . . ?
N4 Ru1 Cl2 89.02(9) . . ?
N1 Ru1 Cl1 86.24(10) . . ?
N3 Ru1 Cl1 172.34(9) . . ?
N2 Ru1 Cl1 100.45(9) . . ?
N4 Ru1 Cl1 99.68(8) . . ?
Cl2 Ru1 Cl1 88.36(4) . . ?
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1537313'
_audit_update_record             
;
2017-05-31 deposited with the CCDC.
2017-06-12 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         
'2(C22 H17 Cl2 N4 O2 Ru), 2(F6 P),C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C50 H47 Cl4 F12 N9 O5 P2 Ru2'
_chemical_formula_weight         1487.85

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.673(2)
_cell_length_b                   25.105(3)
_cell_length_c                   11.5618(12)
_cell_angle_alpha                90
_cell_angle_beta                 97.922(3)
_cell_angle_gamma                90
_cell_volume                     6230.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9827
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      25.32

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             2976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.794
_shelx_estimated_absorpt_T_min   0.870
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            168276
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.897
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12844
_reflns_number_gt                9446
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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)+(0.0707P)²+153.2405P] 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         12844
_refine_ls_number_parameters     826
_refine_ls_number_restraints     279
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0947
_refine_ls_wR_factor_ref         0.2447
_refine_ls_wR_factor_gt          0.2264
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002

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
C1 C 0.8339(6) 0.3910(5) 0.4301(9) 0.044(3) Uani 1 1 d . . . . .
H1 H 0.792755 0.387978 0.448910 0.053 Uiso 1 1 calc R U . . .
C2 C 0.8667(6) 0.4393(6) 0.4539(12) 0.052(3) Uani 1 1 d . . . . .
H2 H 0.848354 0.469090 0.486698 0.063 Uiso 1 1 calc R U . . .
C3 C 0.9260(8) 0.4409(7) 0.4272(16) 0.080(5) Uani 1 1 d . . . . .
H3 H 0.949066 0.473086 0.439061 0.096 Uiso 1 1 calc R U . . .
C4 C 0.9540(7) 0.3963(7) 0.3827(16) 0.071(5) Uani 1 1 d . . . . .
H4 H 0.996262 0.397376 0.369284 0.086 Uiso 1 1 calc R U . . .
C5 C 0.9188(6) 0.3508(5) 0.3588(11) 0.042(3) Uani 1 1 d . . . . .
C6 C 0.9438(5) 0.3016(5) 0.3132(10) 0.042(3) Uani 1 1 d . . . . .
C7 C 1.0017(6) 0.2930(6) 0.2812(12) 0.050(3) Uani 1 1 d . . . . .
H7 H 1.031709 0.320826 0.286995 0.060 Uiso 1 1 calc R U . . .
C8 C 1.0157(5) 0.2426(5) 0.2399(11) 0.043(3) Uani 1 1 d . . . . .
C9 C 0.9729(5) 0.2006(5) 0.2420(10) 0.042(3) Uani 1 1 d . . . . .
H9 H 0.983876 0.165069 0.225004 0.051 Uiso 1 1 calc R U . . .
C10 C 0.9146(5) 0.2124(5) 0.2695(9) 0.036(2) Uani 1 1 d . . . . .
C11 C 0.8624(5) 0.1734(4) 0.2727(9) 0.033(2) Uani 1 1 d . . . . .
C12 C 0.8640(6) 0.1208(5) 0.2432(10) 0.043(3) Uani 1 1 d . . . . .
H12 H 0.900677 0.106263 0.219266 0.051 Uiso 1 1 calc R U . . .
C13 C 0.8129(6) 0.0887(5) 0.2479(11) 0.045(3) Uani 1 1 d . . . . .
H13 H 0.813937 0.052255 0.226370 0.054 Uiso 1 1 calc R U . . .
C14 C 0.7597(5) 0.1105(5) 0.2847(10) 0.041(3) Uani 1 1 d . . . . .
H14 H 0.724097 0.089114 0.290827 0.050 Uiso 1 1 calc R U . . .
C15 C 0.7603(5) 0.1638(4) 0.3118(9) 0.031(2) Uani 1 1 d . . . . .
H15 H 0.724156 0.178905 0.336858 0.037 Uiso 1 1 calc R U . . .
C16 C 1.0761(6) 0.2319(6) 0.1996(13) 0.059(4) Uani 1 1 d . . . . .
C17 C 1.1299(7) 0.2624(7) 0.2380(19) 0.089(7) Uani 1 1 d . . . . .
H17 H 1.127575 0.289866 0.293840 0.107 Uiso 1 1 calc R U . . .
C18 C 1.1861(8) 0.2532(7) 0.196(2) 0.102(8) Uani 1 1 d . . . . .
H18 H 1.221926 0.273667 0.223566 0.122 Uiso 1 1 calc R U . . .
C19 C 1.1892(7) 0.2134(9) 0.1119(15) 0.088(6) Uani 1 1 d . . . . .
C20 C 1.1379(7) 0.1829(9) 0.0747(15) 0.094(7) Uani 1 1 d . . . . .
H20 H 1.140522 0.156016 0.017834 0.112 Uiso 1 1 calc R U . . .
C21 C 1.0814(7) 0.1909(7) 0.1193(12) 0.071(5) Uani 1 1 d . . . . .
H21 H 1.046783 0.168392 0.094882 0.085 Uiso 1 1 calc R U . . .
C22 C 1.2516(8) 0.1664(10) -0.0086(16) 0.104(8) Uani 1 1 d . . . . .
H22A H 1.248641 0.131754 0.029487 0.156 Uiso 1 1 calc R U . . .
H22B H 1.292329 0.169474 -0.035849 0.156 Uiso 1 1 calc R U . . .
H22C H 1.218590 0.169277 -0.075269 0.156 Uiso 1 1 calc R U . . .
C23 C 0.5666(5) 0.4862(3) 0.1045(7) 0.023(2) Uani 1 1 d . . . . .
H23 H 0.595423 0.483734 0.049883 0.028 Uiso 1 1 calc R U . . .
C24 C 0.5405(5) 0.5345(4) 0.1242(8) 0.031(2) Uani 1 1 d . U . . .
H24 H 0.551863 0.565620 0.085428 0.038 Uiso 1 1 calc R U . . .
C25 C 0.4977(5) 0.5370(4) 0.2007(8) 0.031(2) Uani 1 1 d . . . . .
H25 H 0.477157 0.569795 0.210616 0.038 Uiso 1 1 calc R U . . .
C26 C 0.4839(5) 0.4932(3) 0.2638(8) 0.024(2) Uani 1 1 d . U . . .
H26 H 0.455564 0.495591 0.319298 0.029 Uiso 1 1 calc R U . . .
C27 C 0.5128(5) 0.4448(3) 0.2436(7) 0.022(2) Uani 1 1 d . . . . .
C28 C 0.5037(5) 0.3947(3) 0.3063(7) 0.0207(19) Uani 1 1 d . . . . .
C29 C 0.4686(4) 0.3873(4) 0.3949(7) 0.0217(19) Uani 1 1 d . . . . .
H29 H 0.446309 0.416170 0.422289 0.026 Uiso 1 1 calc R U . . .
C30 C 0.4658(4) 0.3357(3) 0.4456(7) 0.0198(18) Uani 1 1 d . . . . .
C31 C 0.4974(4) 0.2938(4) 0.3990(7) 0.0223(19) Uani 1 1 d . . . . .
H31 H 0.495370 0.258839 0.429514 0.027 Uiso 1 1 calc R U . . .
C32 C 0.5315(4) 0.3034(3) 0.3087(7) 0.0177(17) Uani 1 1 d . . . . .
C33 C 0.5645(4) 0.2633(3) 0.2470(7) 0.0180(18) Uani 1 1 d . . . . .
C34 C 0.5644(4) 0.2099(3) 0.2691(7) 0.0181(18) Uani 1 1 d . . . . .
H34 H 0.543879 0.196685 0.330754 0.022 Uiso 1 1 calc R U . . .
C35 C 0.5945(4) 0.1742(4) 0.2009(7) 0.0214(19) Uani 1 1 d . . . . .
H35 H 0.593596 0.136865 0.213897 0.026 Uiso 1 1 calc R U . . .
C36 C 0.6257(4) 0.1957(3) 0.1132(7) 0.0187(18) Uani 1 1 d . . . . .
H36 H 0.647881 0.173230 0.067186 0.022 Uiso 1 1 calc R U . . .
C37 C 0.6237(4) 0.2502(3) 0.0950(7) 0.0193(18) Uani 1 1 d . . . . .
H37 H 0.643552 0.264558 0.033696 0.023 Uiso 1 1 calc R U . . .
C38 C 0.4313(5) 0.3271(3) 0.5443(7) 0.0218(19) Uani 1 1 d . . . . .
C39 C 0.4143(5) 0.3677(4) 0.6152(8) 0.029(2) Uani 1 1 d . . . . .
H39 H 0.423675 0.403609 0.597974 0.035 Uiso 1 1 calc R U . . .
C40 C 0.3840(5) 0.3570(4) 0.7103(9) 0.035(2) Uani 1 1 d . . . . .
H40 H 0.372375 0.385593 0.756548 0.042 Uiso 1 1 calc R U . . .
C41 C 0.3704(5) 0.3058(4) 0.7390(8) 0.030(2) Uani 1 1 d . . . . .
C42 C 0.3869(5) 0.2635(4) 0.6704(9) 0.031(2) Uani 1 1 d . . . . .
H42 H 0.377955 0.227795 0.689960 0.037 Uiso 1 1 calc R U . . .
C43 C 0.4160(5) 0.2740(4) 0.5746(9) 0.027(2) Uani 1 1 d . . . . .
H43 H 0.426116 0.245241 0.527223 0.033 Uiso 1 1 calc R U . . .
C44 C 0.3176(6) 0.3320(6) 0.8990(10) 0.050(3) Uani 1 1 d . . . . .
H44A H 0.352340 0.354008 0.934927 0.075 Uiso 1 1 calc R U . . .
H44B H 0.296268 0.316205 0.960227 0.075 Uiso 1 1 calc R U . . .
H44C H 0.288194 0.354081 0.847821 0.075 Uiso 1 1 calc R U . . .
C45 C 0.8883(8) 0.4214(6) 0.0793(12) 0.065(4) Uani 1 1 d . . . . .
C46 C 0.9349(10) 0.4521(9) 0.0290(18) 0.106(7) Uani 1 1 d . . . . .
H46A H 0.963806 0.427748 -0.002498 0.159 Uiso 1 1 calc R U . . .
H46B H 0.958056 0.474499 0.089504 0.159 Uiso 1 1 calc R U . . .
H46C H 0.914371 0.474682 -0.033944 0.159 Uiso 1 1 calc R U . . .
C47 C 0.2434(12) 0.4776(8) -0.1900(17) 0.107(7) Uani 1 1 d . . . . .
H47A H 0.283281 0.467786 -0.215101 0.161 Uiso 1 1 calc R U . . .
H47B H 0.226079 0.508610 -0.234511 0.161 Uiso 1 1 calc R U . . .
H47C H 0.214332 0.447621 -0.203698 0.161 Uiso 1 1 calc R U . . .
C48 C 0.2539(9) 0.4914(8) -0.0574(17) 0.085(5) Uani 1 1 d . . . . .
H48A H 0.275277 0.526115 -0.043796 0.102 Uiso 1 1 calc R U . . .
H48B H 0.213630 0.493042 -0.026056 0.102 Uiso 1 1 calc R U . . .
C49 C 0.3032(9) 0.4549(8) 0.1233(14) 0.082(5) Uani 1 1 d . . . . .
H49A H 0.330712 0.485806 0.144463 0.099 Uiso 1 1 calc R U . . .
H49B H 0.263208 0.461201 0.153484 0.099 Uiso 1 1 calc R U . . .
C50 C 0.3323(9) 0.4064(9) 0.1751(14) 0.102(8) Uani 1 1 d . . . . .
H50A H 0.300723 0.378536 0.175362 0.153 Uiso 1 1 calc R U . . .
H50B H 0.351300 0.413788 0.255376 0.153 Uiso 1 1 calc R U . . .
H50C H 0.364522 0.394492 0.129174 0.153 Uiso 1 1 calc R U . . .
N1 N 0.7818(4) 0.2965(3) 0.2042(7) 0.0304(19) Uani 1 1 d . . . . .
N2 N 0.8594(4) 0.3495(4) 0.3819(7) 0.034(2) Uani 1 1 d . . . . .
N3 N 0.9008(4) 0.2612(4) 0.3015(7) 0.0322(19) Uani 1 1 d . . . . .
N4 N 0.8088(4) 0.1952(4) 0.3046(7) 0.035(2) Uani 1 1 d . . . . .
N8 N 0.6570(4) 0.3828(3) 0.2247(6) 0.0226(17) Uani 1 1 d . . . . .
N5 N 0.5520(4) 0.4422(3) 0.1610(6) 0.0208(16) Uani 1 1 d . . . . .
N6 N 0.5357(3) 0.3527(3) 0.2700(6) 0.0165(15) Uani 1 1 d . . . . .
N7 N 0.5949(4) 0.2834(3) 0.1601(6) 0.0190(15) Uani 1 1 d . . . . .
N9 N 0.8509(9) 0.3979(7) 0.1194(15) 0.104(6) Uani 1 1 d . . . . .
O1 O 0.7534(4) 0.3129(3) 0.1215(6) 0.0389(18) Uani 1 1 d . . . . .
O2 O 1.2445(5) 0.2098(7) 0.0764(12) 0.109(5) Uani 1 1 d . . . . .
O3 O 0.2921(6) 0.4489(5) -0.0029(10) 0.084(3) Uani 1 1 d . . . . .
O5 O 0.7042(3) 0.3984(3) 0.2659(6) 0.0305(16) Uani 1 1 d . . . . .
O6 O 0.3412(4) 0.2897(3) 0.8307(6) 0.0395(19) Uani 1 1 d . . . . .
P1 P 0.1240(5) 0.4324(4) 0.2623(9) 0.053(2) Uani 0.600(13) 1 d D U P A 1
F1 F 0.1413(9) 0.4664(8) 0.1545(15) 0.074(5) Uani 0.600(13) 1 d D U P A 1
F2 F 0.1745(7) 0.4636(7) 0.3528(15) 0.048(4) Uani 0.600(13) 1 d D U P A 1
F3 F 0.1062(7) 0.3955(6) 0.3677(14) 0.066(4) Uani 0.600(13) 1 d D U P A 1
F4 F 0.0740(8) 0.3983(7) 0.1736(15) 0.086(5) Uani 0.600(13) 1 d D U P A 1
F5 F 0.1751(7) 0.3884(5) 0.2426(14) 0.070(4) Uani 0.600(13) 1 d D U P A 1
F6 F 0.0720(7) 0.4764(8) 0.2806(16) 0.084(5) Uani 0.600(13) 1 d D U P A 1
P1' P 0.1074(8) 0.4476(5) 0.2921(11) 0.054(4) Uani 0.400(13) 1 d D U P A 2
F1' F 0.0922(12) 0.5098(8) 0.286(2) 0.085(7) Uani 0.400(13) 1 d D U P A 2
F2' F 0.0388(10) 0.4327(10) 0.2273(18) 0.080(7) Uani 0.400(13) 1 d D U P A 2
F3' F 0.1251(14) 0.3847(7) 0.299(2) 0.092(7) Uani 0.400(13) 1 d D U P A 2
F4' F 0.1789(12) 0.4603(16) 0.347(3) 0.100(10) Uani 0.400(13) 1 d D U P A 2
F5' F 0.1308(15) 0.4489(11) 0.166(2) 0.084(7) Uani 0.400(13) 1 d D U P A 2
F6' F 0.0849(11) 0.4463(9) 0.4190(15) 0.082(7) Uani 0.400(13) 1 d D U P A 2
F7 F 0.6246(3) 0.4132(2) 0.4524(5) 0.0365(14) Uani 1 1 d . . . . .
F8 F 0.6440(3) 0.4925(2) 0.3747(5) 0.0400(15) Uani 1 1 d . . . . .
F9 F 0.6599(4) 0.5283(2) 0.5570(6) 0.0513(19) Uani 1 1 d . . . . .
F10 F 0.6399(3) 0.4489(2) 0.6337(5) 0.0403(15) Uani 1 1 d . . . . .
F11 F 0.5710(3) 0.4865(3) 0.4942(5) 0.0439(16) Uani 1 1 d . . . . .
F12 F 0.7149(3) 0.4563(3) 0.5152(6) 0.0443(16) Uani 1 1 d . . . . .
P2 P 0.64336(13) 0.47080(10) 0.5049(2) 0.0273(6) Uani 1 1 d . . . . .
Cl2 Cl 0.86164(14) 0.24990(12) 0.5273(2) 0.0424(7) Uani 1 1 d . . . . .
Cl1 Cl 0.71957(13) 0.28831(11) 0.4084(2) 0.0384(6) Uani 1 1 d . . . . .
Cl4 Cl 0.49328(11) 0.34724(8) 0.01801(17) 0.0208(4) Uani 1 1 d . . . . .
Cl3 Cl 0.63505(11) 0.38028(8) -0.02808(18) 0.0238(5) Uani 1 1 d . . . . .
Ru1 Ru 0.81779(4) 0.27555(3) 0.34170(7) 0.0287(2) Uani 1 1 d . . . . .
Ru2 Ru 0.58606(4) 0.36582(3) 0.14180(6) 0.01762(18) 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
C1 N2 1.337(15) . ?
C1 C2 1.413(18) . ?
C1 H1 0.9500 . ?
C2 C3 1.36(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.41(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(18) . ?
C4 H4 0.9500 . ?
C5 N2 1.352(15) . ?
C5 C6 1.475(16) . ?
C6 C7 1.372(16) . ?
C6 N3 1.372(14) . ?
C7 C8 1.401(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.408(17) . ?
C8 C16 1.474(17) . ?
C9 C10 1.377(15) . ?
C9 H9 0.9500 . ?
C10 N3 1.326(14) . ?
C10 C11 1.500(16) . ?
C11 C12 1.364(16) . ?
C11 N4 1.380(14) . ?
C12 C13 1.376(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.374(16) . ?
C14 H14 0.9500 . ?
C15 N4 1.326(14) . ?
C15 H15 0.9500 . ?
C16 C21 1.40(2) . ?
C16 C17 1.415(19) . ?
C17 C18 1.39(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.40(2) . ?
C18 H18 0.9500 . ?
C19 O2 1.322(17) . ?
C19 C20 1.37(2) . ?
C20 C21 1.41(2) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O2 1.49(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 N5 1.341(11) . ?
C23 C24 1.371(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.376(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(12) . ?
C26 H26 0.9500 . ?
C27 N5 1.365(12) . ?
C27 C28 1.480(11) . ?
C28 N6 1.360(11) . ?
C28 C29 1.370(12) . ?
C29 C30 1.425(12) . ?
C29 H29 0.9500 . ?
C30 C31 1.403(12) . ?
C30 C38 1.464(12) . ?
C31 C32 1.379(12) . ?
C31 H31 0.9500 . ?
C32 N6 1.325(11) . ?
C32 C33 1.475(12) . ?
C33 C34 1.365(12) . ?
C33 N7 1.371(11) . ?
C34 C35 1.412(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.401(12) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(12) . ?
C36 H36 0.9500 . ?
C37 N7 1.334(11) . ?
C37 H37 0.9500 . ?
C38 C39 1.389(13) . ?
C38 C43 1.430(13) . ?
C39 C40 1.383(13) . ?
C39 H39 0.9500 . ?
C40 C41 1.369(15) . ?
C40 H40 0.9500 . ?
C41 O6 1.369(12) . ?
C41 C42 1.401(14) . ?
C42 C43 1.374(13) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 O6 1.458(14) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 N9 1.15(2) . ?
C45 C46 1.45(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.56(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O3 1.441(19) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.46(2) . ?
C49 O3 1.454(19) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N1 O1 1.142(11) . ?
N1 Ru1 1.751(9) . ?
N2 Ru1 2.087(9) . ?
N3 Ru1 1.952(9) . ?
N4 Ru1 2.067(10) . ?
N8 O5 1.135(10) . ?
N8 Ru2 1.749(8) . ?
N5 Ru2 2.078(7) . ?
N6 Ru2 1.985(7) . ?
N7 Ru2 2.086(7) . ?
P1 F5 1.602(16) . ?
P1 F1 1.598(14) . ?
P1 F3 1.618(13) . ?
P1 F6 1.614(16) . ?
P1 F2 1.609(18) . ?
P1 F4 1.629(18) . ?
P1' F1' 1.597(18) . ?
P1' F5' 1.61(2) . ?
P1' F6' 1.609(18) . ?
P1' F3' 1.624(16) . ?
P1' F4' 1.63(2) . ?
P1' F2' 1.61(2) . ?
F7 P2 1.600(6) . ?
F8 P2 1.603(6) . ?
F9 P2 1.585(6) . ?
F10 P2 1.599(6) . ?
F11 P2 1.606(7) . ?
F12 P2 1.581(7) . ?
Cl2 Ru1 2.316(3) . ?
Cl1 Ru1 2.384(3) . ?
Cl4 Ru2 2.349(2) . ?
Cl3 Ru2 2.386(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
N2 C1 C2 121.7(12) . . ?
N2 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 116.5(12) . . ?
C3 C2 H2 121.8 . . ?
C1 C2 H2 121.8 . . ?
C2 C3 C4 121.8(14) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 118.6(13) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N2 C5 C4 119.8(11) . . ?
N2 C5 C6 117.2(10) . . ?
C4 C5 C6 123.0(12) . . ?
C7 C6 N3 119.5(11) . . ?
C7 C6 C5 128.5(12) . . ?
N3 C6 C5 112.0(10) . . ?
C6 C7 C8 118.9(12) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 119.8(11) . . ?
C9 C8 C16 119.0(11) . . ?
C7 C8 C16 121.2(11) . . ?
C10 C9 C8 118.0(11) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N3 C10 C9 120.9(11) . . ?
N3 C10 C11 113.4(10) . . ?
C9 C10 C11 125.6(11) . . ?
C12 C11 N4 120.1(11) . . ?
C12 C11 C10 125.5(11) . . ?
N4 C11 C10 114.4(9) . . ?
C11 C12 C13 120.6(11) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.1(11) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 117.9(11) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
N4 C15 C14 123.1(11) . . ?
N4 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C21 C16 C17 117.8(13) . . ?
C21 C16 C8 120.1(12) . . ?
C17 C16 C8 122.0(13) . . ?
C18 C17 C16 121.5(15) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.3(16) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
O2 C19 C20 126.6(17) . . ?
O2 C19 C18 113.3(16) . . ?
C20 C19 C18 120.1(14) . . ?
C19 C20 C21 121.1(16) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C20 120.1(14) . . ?
C16 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
O2 C22 H22A 109.5 . . ?
O2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 C24 121.1(9) . . ?
N5 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 C23 118.7(9) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 121.4(9) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C27 118.1(9) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
N5 C27 C26 119.6(8) . . ?
N5 C27 C28 116.1(8) . . ?
C26 C27 C28 124.2(9) . . ?
N6 C28 C29 119.0(8) . . ?
N6 C28 C27 113.5(8) . . ?
C29 C28 C27 127.4(8) . . ?
C28 C29 C30 119.4(8) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C31 C30 C29 118.2(8) . . ?
C31 C30 C38 121.2(8) . . ?
C29 C30 C38 120.6(8) . . ?
C32 C31 C30 120.0(8) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
N6 C32 C31 119.2(8) . . ?
N6 C32 C33 114.4(7) . . ?
C31 C32 C33 126.4(8) . . ?
C34 C33 N7 120.8(8) . . ?
C34 C33 C32 124.4(8) . . ?
N7 C33 C32 114.7(7) . . ?
C33 C34 C35 120.4(8) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 117.8(8) . . ?
C36 C35 H35 121.1 . . ?
C34 C35 H35 121.1 . . ?
C37 C36 C35 118.8(8) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
N7 C37 C36 122.7(8) . . ?
N7 C37 H37 118.7 . . ?
C36 C37 H37 118.7 . . ?
C39 C38 C43 116.8(8) . . ?
C39 C38 C30 123.9(8) . . ?
C43 C38 C30 119.3(8) . . ?
C40 C39 C38 121.3(9) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C41 C40 C39 121.1(9) . . ?
C41 C40 H40 119.4 . . ?
C39 C40 H40 119.4 . . ?
C40 C41 O6 127.1(9) . . ?
C40 C41 C42 119.7(9) . . ?
O6 C41 C42 113.3(9) . . ?
C43 C42 C41 119.4(10) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C38 121.7(9) . . ?
C42 C43 H43 119.2 . . ?
C38 C43 H43 119.2 . . ?
O6 C44 H44A 109.5 . . ?
O6 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O6 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N9 C45 C46 179(2) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C48 C47 105.2(15) . . ?
O3 C48 H48A 110.7 . . ?
C47 C48 H48A 110.7 . . ?
O3 C48 H48B 110.7 . . ?
C47 C48 H48B 110.7 . . ?
H48A C48 H48B 108.8 . . ?
C50 C49 O3 109.2(14) . . ?
C50 C49 H49A 109.9 . . ?
O3 C49 H49A 109.9 . . ?
C50 C49 H49B 109.8 . . ?
O3 C49 H49B 109.8 . . ?
H49A C49 H49B 108.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O1 N1 Ru1 172.0(8) . . ?
C1 N2 C5 121.5(10) . . ?
C1 N2 Ru1 126.6(8) . . ?
C5 N2 Ru1 111.8(7) . . ?
C10 N3 C6 122.2(10) . . ?
C10 N3 Ru1 119.2(8) . . ?
C6 N3 Ru1 118.5(8) . . ?
C15 N4 C11 119.1(10) . . ?
C15 N4 Ru1 128.3(7) . . ?
C11 N4 Ru1 112.6(7) . . ?
O5 N8 Ru2 170.5(7) . . ?
C23 N5 C27 120.8(8) . . ?
C23 N5 Ru2 126.6(6) . . ?
C27 N5 Ru2 112.5(5) . . ?
C32 N6 C28 123.9(8) . . ?
C32 N6 Ru2 118.6(6) . . ?
C28 N6 Ru2 117.3(6) . . ?
C37 N7 C33 119.5(7) . . ?
C37 N7 Ru2 127.3(6) . . ?
C33 N7 Ru2 113.1(6) . . ?
C19 O2 C22 115.8(15) . . ?
C48 O3 C49 111.6(14) . . ?
C41 O6 C44 116.0(9) . . ?
F5 P1 F1 91.0(11) . . ?
F5 P1 F3 87.4(9) . . ?
F1 P1 F3 177.4(14) . . ?
F5 P1 F6 179.2(13) . . ?
F1 P1 F6 88.8(11) . . ?
F3 P1 F6 92.9(10) . . ?
F5 P1 F2 90.4(9) . . ?
F1 P1 F2 92.0(10) . . ?
F3 P1 F2 90.0(10) . . ?
F6 P1 F2 90.3(11) . . ?
F5 P1 F4 87.8(10) . . ?
F1 P1 F4 89.9(10) . . ?
F3 P1 F4 88.1(9) . . ?
F6 P1 F4 91.5(11) . . ?
F2 P1 F4 177.4(11) . . ?
F1' P1' F5' 91.6(14) . . ?
F1' P1' F6' 88.5(14) . . ?
F5' P1' F6' 179.2(17) . . ?
F1' P1' F3' 178.2(19) . . ?
F5' P1' F3' 87.7(15) . . ?
F6' P1' F3' 92.2(13) . . ?
F1' P1' F4' 90.2(16) . . ?
F5' P1' F4' 87.1(18) . . ?
F6' P1' F4' 92.2(17) . . ?
F3' P1' F4' 88.1(17) . . ?
F1' P1' F2' 92.0(14) . . ?
F5' P1' F2' 88.3(14) . . ?
F6' P1' F2' 92.5(13) . . ?
F3' P1' F2' 89.6(14) . . ?
F4' P1' F2' 174.9(19) . . ?
F12 P2 F9 90.7(4) . . ?
F12 P2 F10 91.3(4) . . ?
F9 P2 F10 89.8(4) . . ?
F12 P2 F7 90.9(4) . . ?
F9 P2 F7 178.4(4) . . ?
F10 P2 F7 90.0(3) . . ?
F12 P2 F8 90.8(4) . . ?
F9 P2 F8 90.9(4) . . ?
F10 P2 F8 177.8(4) . . ?
F7 P2 F8 89.2(3) . . ?
F12 P2 F11 179.1(4) . . ?
F9 P2 F11 88.5(4) . . ?
F10 P2 F11 89.2(4) . . ?
F7 P2 F11 89.9(4) . . ?
F8 P2 F11 88.7(4) . . ?
N1 Ru1 N3 98.6(4) . . ?
N1 Ru1 N4 95.0(4) . . ?
N3 Ru1 N4 80.4(4) . . ?
N1 Ru1 N2 93.4(4) . . ?
N3 Ru1 N2 80.4(4) . . ?
N4 Ru1 N2 160.0(4) . . ?
N1 Ru1 Cl2 177.3(3) . . ?
N3 Ru1 Cl2 84.0(3) . . ?
N4 Ru1 Cl2 86.3(2) . . ?
N2 Ru1 Cl2 86.1(3) . . ?
N1 Ru1 Cl1 87.0(3) . . ?
N3 Ru1 Cl1 174.3(3) . . ?
N4 Ru1 Cl1 97.8(2) . . ?
N2 Ru1 Cl1 100.7(3) . . ?
Cl2 Ru1 Cl1 90.46(10) . . ?
N8 Ru2 N6 99.5(3) . . ?
N8 Ru2 N5 90.8(3) . . ?
N6 Ru2 N5 80.4(3) . . ?
N8 Ru2 N7 97.2(3) . . ?
N6 Ru2 N7 79.2(3) . . ?
N5 Ru2 N7 159.0(3) . . ?
N8 Ru2 Cl4 175.3(2) . . ?
N6 Ru2 Cl4 84.8(2) . . ?
N5 Ru2 Cl4 87.8(2) . . ?
N7 Ru2 Cl4 85.6(2) . . ?
N8 Ru2 Cl3 87.5(2) . . ?
N6 Ru2 Cl3 173.0(2) . . ?
N5 Ru2 Cl3 98.8(2) . . ?
N7 Ru2 Cl3 100.9(2) . . ?
Cl4 Ru2 Cl3 88.24(8) . . ?

_refine_diff_density_max         1.916
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.189



