# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_msb577_0m
_database_code_depnum_ccdc_archive 'CCDC 1408417'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
2-(diphenylphosphanyl)-1-{[2-(diphenylphosphanyl)-1H-imidazole]methyl}-1H-imidazole
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 N4 P2'
_chemical_formula_sum            'C31 H26 N4 P2'
_chemical_formula_weight         516.50

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   8.9713(7)
_cell_length_b                   10.3845(8)
_cell_length_c                   27.663(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2577.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1482
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      27.80

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7060
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 20 sec/frame. Analysis of 1241 reflections
 having I/σ(I) > 15 and chosen from the full data set with
 CELL_NOW (Sheldrick, 2008a) showed the crystal to belong to the
 orthorhombic system and to contain a minor component rotated by
 175° about b.  The raw data were processed using the
 multi-component version of SAINT under control of the 
 two-component orientation file generated by CELL_NOW.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83301
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         28.22
_reflns_number_total             6350
_reflns_number_gt                6085
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2008)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'

_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. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms. The final refinement was performed with the
 single-component (major) reflection file extracted from the full data set
 with TWINABS. 
;

_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)+(0.0420P)²+0.8639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack, 1983'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_number_reflns         6350
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0828
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 1.00870(5) 0.35774(4) 0.121117(14) 0.01869(9) Uani 1 1 d . . .
P2 P 1.03282(4) 0.86343(4) 0.065535(14) 0.01512(8) Uani 1 1 d . . .
N1 N 1.10284(18) 0.52711(15) 0.19526(5) 0.0237(3) Uani 1 1 d . . .
N2 N 1.16799(14) 0.59065(13) 0.12128(5) 0.0153(3) Uani 1 1 d . . .
N3 N 1.07462(14) 0.60751(12) 0.03828(5) 0.0147(3) Uani 1 1 d . . .
N4 N 0.90050(16) 0.70365(13) -0.00606(5) 0.0180(3) Uani 1 1 d . . .
C1 C 1.10254(19) 0.22967(16) 0.15471(6) 0.0188(3) Uani 1 1 d . . .
C2 C 1.19298(17) 0.14541(17) 0.12865(6) 0.0207(3) Uani 1 1 d . . .
H2 H 1.1984 0.1526 0.0945 0.025 Uiso 1 1 calc R . .
C3 C 1.2755(2) 0.05084(18) 0.15226(7) 0.0245(4) Uani 1 1 d . . .
H3 H 1.3393 -0.0045 0.1344 0.029 Uiso 1 1 calc R . .
C4 C 1.2642(2) 0.03797(17) 0.20180(7) 0.0250(4) Uani 1 1 d . . .
H4 H 1.3200 -0.0267 0.2180 0.030 Uiso 1 1 calc R . .
C5 C 1.1718(2) 0.11889(18) 0.22809(6) 0.0255(4) Uani 1 1 d . . .
H5 H 1.1631 0.1084 0.2621 0.031 Uiso 1 1 calc R . .
C6 C 1.0921(2) 0.21523(17) 0.20476(6) 0.0220(3) Uani 1 1 d . . .
H6 H 1.0303 0.2715 0.2229 0.026 Uiso 1 1 calc R . .
C7 C 0.82512(18) 0.36415(18) 0.15018(6) 0.0195(3) Uani 1 1 d . . .
C8 C 0.7504(2) 0.24940(18) 0.16075(7) 0.0241(4) Uani 1 1 d . . .
H8 H 0.7997 0.1694 0.1560 0.029 Uiso 1 1 calc R . .
C9 C 0.6045(2) 0.2507(2) 0.17810(7) 0.0295(4) Uani 1 1 d . . .
H9 H 0.5553 0.1720 0.1852 0.035 Uiso 1 1 calc R . .
C10 C 0.5310(2) 0.3671(2) 0.18499(6) 0.0320(4) Uani 1 1 d . . .
H10 H 0.4315 0.3683 0.1968 0.038 Uiso 1 1 calc R . .
C11 C 0.6042(2) 0.4817(2) 0.17450(7) 0.0290(4) Uani 1 1 d . . .
H11 H 0.5547 0.5615 0.1794 0.035 Uiso 1 1 calc R . .
C12 C 0.7496(2) 0.48030(18) 0.15689(6) 0.0232(4) Uani 1 1 d . . .
H12 H 0.7978 0.5592 0.1494 0.028 Uiso 1 1 calc R . .
C13 C 1.09650(18) 0.49805(16) 0.14854(6) 0.0178(3) Uani 1 1 d . . .
C14 C 1.18087(18) 0.64071(18) 0.19805(6) 0.0218(3) Uani 1 1 d . . .
H14 H 1.2030 0.6850 0.2272 0.026 Uiso 1 1 calc R . .
C15 C 1.22197(18) 0.68102(16) 0.15318(6) 0.0192(3) Uani 1 1 d . . .
H15 H 1.2769 0.7564 0.1454 0.023 Uiso 1 1 calc R . .
C16 C 1.20274(16) 0.58786(15) 0.06969(5) 0.0152(3) Uani 1 1 d . . .
H16A H 1.2776 0.6555 0.0627 0.018 Uiso 1 1 calc R . .
H16B H 1.2485 0.5037 0.0618 0.018 Uiso 1 1 calc R . .
C17 C 1.02028(17) 0.51617(15) 0.00710(5) 0.0170(3) Uani 1 1 d . . .
H17 H 1.0507 0.4288 0.0047 0.020 Uiso 1 1 calc R . .
C18 C 0.91377(18) 0.57642(16) -0.01980(6) 0.0183(3) Uani 1 1 d . . .
H18 H 0.8567 0.5364 -0.0445 0.022 Uiso 1 1 calc R . .
C19 C 0.99907(17) 0.72038(14) 0.02909(5) 0.0152(3) Uani 1 1 d . . .
C20 C 0.87249(17) 0.85740(16) 0.10658(5) 0.0166(3) Uani 1 1 d . . .
C21 C 0.73048(19) 0.81939(17) 0.09165(6) 0.0210(3) Uani 1 1 d . . .
H21 H 0.7136 0.7969 0.0588 0.025 Uiso 1 1 calc R . .
C22 C 0.6140(2) 0.81434(18) 0.12454(7) 0.0263(4) Uani 1 1 d . . .
H22 H 0.5180 0.7870 0.1143 0.032 Uiso 1 1 calc R . .
C23 C 0.6377(2) 0.84939(19) 0.17252(6) 0.0278(4) Uani 1 1 d . . .
H23 H 0.5576 0.8461 0.1950 0.033 Uiso 1 1 calc R . .
C24 C 0.7774(2) 0.88899(17) 0.18761(6) 0.0244(4) Uani 1 1 d . . .
H24 H 0.7930 0.9136 0.2203 0.029 Uiso 1 1 calc R . .
C25 C 0.89531(19) 0.89276(15) 0.15480(6) 0.0200(3) Uani 1 1 d . . .
H25 H 0.9914 0.9194 0.1652 0.024 Uiso 1 1 calc R . .
C26 C 0.98182(17) 0.99070(14) 0.02280(5) 0.0154(3) Uani 1 1 d . . .
C27 C 0.88235(18) 1.08871(15) 0.03493(6) 0.0185(3) Uani 1 1 d . . .
H27 H 0.8279 1.0837 0.0643 0.022 Uiso 1 1 calc R . .
C28 C 0.86211(19) 1.19385(16) 0.00440(6) 0.0218(3) Uani 1 1 d . . .
H28 H 0.7942 1.2601 0.0130 0.026 Uiso 1 1 calc R . .
C29 C 0.94133(18) 1.20190(16) -0.03873(6) 0.0208(3) Uani 1 1 d . . .
H29 H 0.9277 1.2737 -0.0596 0.025 Uiso 1 1 calc R . .
C30 C 1.04041(18) 1.10480(15) -0.05124(6) 0.0195(3) Uani 1 1 d . . .
H30 H 1.0944 1.1101 -0.0807 0.023 Uiso 1 1 calc R . .
C31 C 1.06095(17) 0.99967(16) -0.02074(6) 0.0175(3) Uani 1 1 d . . .
H31 H 1.1290 0.9336 -0.0295 0.021 Uiso 1 1 calc R . .


_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
P1 C13 1.8219(17) . ?
P1 C1 1.8279(17) . ?
P1 C7 1.8339(17) . ?
P2 C19 1.8206(15) . ?
P2 C26 1.8314(15) . ?
P2 C20 1.8335(15) . ?
N1 C13 1.328(2) . ?
N1 C14 1.374(2) . ?
N2 C15 1.376(2) . ?
N2 C13 1.380(2) . ?
N2 C16 1.461(2) . ?
N3 C17 1.3716(19) . ?
N3 C19 1.3776(19) . ?
N3 C16 1.4553(19) . ?
N4 C19 1.326(2) . ?
N4 C18 1.380(2) . ?
C1 C2 1.394(2) . ?
C1 C6 1.396(2) . ?
C2 C3 1.393(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.396(3) . ?
C7 C8 1.398(2) . ?
C8 C9 1.394(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.361(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.363(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C20 C21 1.396(2) . ?
C20 C25 1.399(2) . ?
C21 C22 1.387(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.393(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(2) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.395(2) . ?
C26 C31 1.401(2) . ?
C27 C28 1.392(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.391(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.392(2) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
C13 P1 C1 99.85(7) . . ?
C13 P1 C7 100.18(8) . . ?
C1 P1 C7 102.55(8) . . ?
C19 P2 C26 100.94(7) . . ?
C19 P2 C20 100.64(7) . . ?
C26 P2 C20 103.20(7) . . ?
C13 N1 C14 105.75(14) . . ?
C15 N2 C13 106.75(13) . . ?
C15 N2 C16 124.39(13) . . ?
C13 N2 C16 128.26(14) . . ?
C17 N3 C19 107.31(12) . . ?
C17 N3 C16 124.00(13) . . ?
C19 N3 C16 128.17(13) . . ?
C19 N4 C18 105.66(13) . . ?
C2 C1 C6 118.98(16) . . ?
C2 C1 P1 117.50(12) . . ?
C6 C1 P1 123.48(14) . . ?
C3 C2 C1 120.62(15) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 119.65(17) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.41(17) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.05(16) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.25(17) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C12 C7 C8 118.41(15) . . ?
C12 C7 P1 121.72(14) . . ?
C8 C7 P1 119.42(14) . . ?
C9 C8 C7 120.90(18) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C10 C9 C8 120.10(18) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.44(17) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.45(19) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.69(18) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
N1 C13 N2 110.70(14) . . ?
N1 C13 P1 127.25(13) . . ?
N2 C13 P1 122.04(12) . . ?
C15 C14 N1 110.55(15) . . ?
C15 C14 H14 124.7 . . ?
N1 C14 H14 124.7 . . ?
C14 C15 N2 106.25(15) . . ?
C14 C15 H15 126.9 . . ?
N2 C15 H15 126.9 . . ?
N3 C16 N2 114.33(12) . . ?
N3 C16 H16A 108.7 . . ?
N2 C16 H16A 108.7 . . ?
N3 C16 H16B 108.7 . . ?
N2 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 N3 105.96(13) . . ?
C18 C17 H17 127.0 . . ?
N3 C17 H17 127.0 . . ?
C17 C18 N4 110.47(14) . . ?
C17 C18 H18 124.8 . . ?
N4 C18 H18 124.8 . . ?
N4 C19 N3 110.60(13) . . ?
N4 C19 P2 128.61(12) . . ?
N3 C19 P2 120.68(11) . . ?
C21 C20 C25 119.32(15) . . ?
C21 C20 P2 122.85(12) . . ?
C25 C20 P2 117.83(12) . . ?
C22 C21 C20 120.30(16) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 120.03(17) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.22(16) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.96(16) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 120.16(16) . . ?
C24 C25 H25 119.9 . . ?
C20 C25 H25 119.9 . . ?
C27 C26 C31 118.86(14) . . ?
C27 C26 P2 122.09(12) . . ?
C31 C26 P2 118.44(12) . . ?
C28 C27 C26 120.65(15) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 120.04(15) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.83(15) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.22(15) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C26 120.40(15) . . ?
C30 C31 H31 119.8 . . ?
C26 C31 H31 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 P1 C1 C2 -116.26(14) . . . . ?
C7 P1 C1 C2 140.89(13) . . . . ?
C13 P1 C1 C6 61.47(16) . . . . ?
C7 P1 C1 C6 -41.38(16) . . . . ?
C6 C1 C2 C3 -2.0(2) . . . . ?
P1 C1 C2 C3 175.79(13) . . . . ?
C1 C2 C3 C4 1.9(3) . . . . ?
C2 C3 C4 C5 -0.3(3) . . . . ?
C3 C4 C5 C6 -1.2(3) . . . . ?
C4 C5 C6 C1 1.1(3) . . . . ?
C2 C1 C6 C5 0.5(3) . . . . ?
P1 C1 C6 C5 -177.18(13) . . . . ?
C13 P1 C7 C12 41.26(15) . . . . ?
C1 P1 C7 C12 143.85(14) . . . . ?
C13 P1 C7 C8 -146.51(14) . . . . ?
C1 P1 C7 C8 -43.93(15) . . . . ?
C12 C7 C8 C9 -0.7(3) . . . . ?
P1 C7 C8 C9 -173.20(14) . . . . ?
C7 C8 C9 C10 0.2(3) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
C9 C10 C11 C12 0.5(3) . . . . ?
C10 C11 C12 C7 -1.0(3) . . . . ?
C8 C7 C12 C11 1.1(2) . . . . ?
P1 C7 C12 C11 173.41(13) . . . . ?
C14 N1 C13 N2 -0.29(19) . . . . ?
C14 N1 C13 P1 179.56(13) . . . . ?
C15 N2 C13 N1 0.42(19) . . . . ?
C16 N2 C13 N1 171.66(15) . . . . ?
C15 N2 C13 P1 -179.44(12) . . . . ?
C16 N2 C13 P1 -8.2(2) . . . . ?
C1 P1 C13 N1 -54.75(17) . . . . ?
C7 P1 C13 N1 50.03(17) . . . . ?
C1 P1 C13 N2 125.08(14) . . . . ?
C7 P1 C13 N2 -130.14(14) . . . . ?
C13 N1 C14 C15 0.1(2) . . . . ?
N1 C14 C15 N2 0.20(19) . . . . ?
C13 N2 C15 C14 -0.36(18) . . . . ?
C16 N2 C15 C14 -172.03(14) . . . . ?
C17 N3 C16 N2 -115.20(16) . . . . ?
C19 N3 C16 N2 74.11(19) . . . . ?
C15 N2 C16 N3 -116.25(16) . . . . ?
C13 N2 C16 N3 73.9(2) . . . . ?
C19 N3 C17 C18 -0.11(17) . . . . ?
C16 N3 C17 C18 -172.45(13) . . . . ?
N3 C17 C18 N4 0.03(18) . . . . ?
C19 N4 C18 C17 0.07(18) . . . . ?
C18 N4 C19 N3 -0.14(18) . . . . ?
C18 N4 C19 P2 -176.37(12) . . . . ?
C17 N3 C19 N4 0.16(17) . . . . ?
C16 N3 C19 N4 172.08(14) . . . . ?
C17 N3 C19 P2 176.74(11) . . . . ?
C16 N3 C19 P2 -11.3(2) . . . . ?
C26 P2 C19 N4 -30.06(15) . . . . ?
C20 P2 C19 N4 75.78(15) . . . . ?
C26 P2 C19 N3 154.04(13) . . . . ?
C20 P2 C19 N3 -100.12(13) . . . . ?
C19 P2 C20 C21 -38.49(16) . . . . ?
C26 P2 C20 C21 65.54(16) . . . . ?
C19 P2 C20 C25 141.53(13) . . . . ?
C26 P2 C20 C25 -114.44(13) . . . . ?
C25 C20 C21 C22 -1.3(3) . . . . ?
P2 C20 C21 C22 178.76(13) . . . . ?
C20 C21 C22 C23 1.1(3) . . . . ?
C21 C22 C23 C24 -0.2(3) . . . . ?
C22 C23 C24 C25 -0.6(3) . . . . ?
C23 C24 C25 C20 0.4(3) . . . . ?
C21 C20 C25 C24 0.5(2) . . . . ?
P2 C20 C25 C24 -179.52(12) . . . . ?
C19 P2 C26 C27 128.82(14) . . . . ?
C20 P2 C26 C27 25.03(15) . . . . ?
C19 P2 C26 C31 -60.29(13) . . . . ?
C20 P2 C26 C31 -164.08(12) . . . . ?
C31 C26 C27 C28 -0.1(2) . . . . ?
P2 C26 C27 C28 170.72(13) . . . . ?
C26 C27 C28 C29 0.1(2) . . . . ?
C27 C28 C29 C30 0.1(2) . . . . ?
C28 C29 C30 C31 -0.2(2) . . . . ?
C29 C30 C31 C26 0.1(2) . . . . ?
C27 C26 C31 C30 0.0(2) . . . . ?
P2 C26 C31 C30 -171.14(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.22
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.047

####################################################################### 
# 
# 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_msb621_0m
_database_code_depnum_ccdc_archive 'CCDC 1408420'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'5-(Diphenylphosphanyl)-1-{[5-(diphosphanyl)-1H-pyrazol-1-yl]methyl}-1H-pyrazole chloroform solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 N4 P2, C H Cl3'
_chemical_formula_sum            'C32 H27 Cl3 N4 P2'
_chemical_formula_weight         635.87

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.323(2)
_cell_length_b                   12.892(2)
_cell_length_c                   12.951(2)
_cell_angle_alpha                93.945(2)
_cell_angle_beta                 117.423(2)
_cell_angle_gamma                117.267(2)
_cell_volume                     1517.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9018
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      28.38

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9177
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26708
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         28.40
_reflns_number_total             7461
_reflns_number_gt                6592
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'

_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. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms.
;

_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)+(0.0387P)²+0.6457P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7461
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.76959(4) 0.73054(3) -0.03009(3) 0.01626(8) Uani 1 1 d . . .
P2 P 1.19878(4) 0.97205(3) 0.22713(3) 0.01715(8) Uani 1 1 d . . .
N1 N 0.83540(12) 0.45461(10) 0.00413(10) 0.0173(2) Uani 1 1 d . . .
N2 N 0.87282(11) 0.57450(9) 0.02439(10) 0.0152(2) Uani 1 1 d . . .
N3 N 1.08200(12) 0.72748(10) 0.22643(10) 0.0158(2) Uani 1 1 d . . .
N4 N 1.06690(13) 0.65225(10) 0.29390(11) 0.0206(2) Uani 1 1 d . . .
C1 C 0.79602(14) 0.78304(12) 0.11979(12) 0.0178(3) Uani 1 1 d . . .
C2 C 0.84129(15) 0.90681(13) 0.16623(14) 0.0229(3) Uani 1 1 d . . .
H2 H 0.8584 0.9603 0.1208 0.027 Uiso 1 1 calc R . .
C3 C 0.86133(16) 0.95176(14) 0.27870(15) 0.0277(3) Uani 1 1 d . . .
H3 H 0.8905 1.0354 0.3089 0.033 Uiso 1 1 calc R . .
C4 C 0.83902(16) 0.87541(15) 0.34665(14) 0.0283(3) Uani 1 1 d . . .
H4 H 0.8523 0.9064 0.4231 0.034 Uiso 1 1 calc R . .
C5 C 0.79718(16) 0.75333(14) 0.30279(14) 0.0261(3) Uani 1 1 d . . .
H5 H 0.7833 0.7011 0.3499 0.031 Uiso 1 1 calc R . .
C6 C 0.77560(15) 0.70751(13) 0.18995(13) 0.0213(3) Uani 1 1 d . . .
H6 H 0.7466 0.6238 0.1603 0.026 Uiso 1 1 calc R . .
C7 C 0.57411(14) 0.66594(11) -0.14148(12) 0.0161(2) Uani 1 1 d . . .
C8 C 0.52182(15) 0.63560(12) -0.26795(13) 0.0202(3) Uani 1 1 d . . .
H8 H 0.5872 0.6491 -0.2928 0.024 Uiso 1 1 calc R . .
C9 C 0.37526(16) 0.58603(13) -0.35720(13) 0.0228(3) Uani 1 1 d . . .
H9 H 0.3403 0.5641 -0.4429 0.027 Uiso 1 1 calc R . .
C10 C 0.27924(16) 0.56832(13) -0.32121(13) 0.0234(3) Uani 1 1 d . . .
H10 H 0.1790 0.5348 -0.3823 0.028 Uiso 1 1 calc R . .
C11 C 0.33054(15) 0.59974(13) -0.19610(13) 0.0223(3) Uani 1 1 d . . .
H11 H 0.2653 0.5883 -0.1715 0.027 Uiso 1 1 calc R . .
C12 C 0.47693(15) 0.64789(12) -0.10640(13) 0.0191(3) Uani 1 1 d . . .
H12 H 0.5111 0.6686 -0.0209 0.023 Uiso 1 1 calc R . .
C13 C 0.75368(14) 0.58258(11) -0.03349(12) 0.0153(2) Uani 1 1 d . . .
C14 C 0.63246(14) 0.46062(12) -0.09573(12) 0.0174(3) Uani 1 1 d . . .
H14 H 0.5322 0.4332 -0.1456 0.021 Uiso 1 1 calc R . .
C15 C 0.68940(15) 0.38615(12) -0.06939(12) 0.0185(3) Uani 1 1 d . . .
H15 H 0.6308 0.2975 -0.1003 0.022 Uiso 1 1 calc R . .
C16 C 1.02680(14) 0.67394(11) 0.09683(12) 0.0168(2) Uani 1 1 d . . .
H16A H 1.0416 0.7403 0.0603 0.020 Uiso 1 1 calc R . .
H16B H 1.0837 0.6410 0.0925 0.020 Uiso 1 1 calc R . .
C17 C 1.13603(16) 0.73072(13) 0.40790(13) 0.0235(3) Uani 1 1 d . . .
H17 H 1.1430 0.7053 0.4766 0.028 Uiso 1 1 calc R . .
C18 C 1.19737(15) 0.85554(13) 0.41461(13) 0.0223(3) Uani 1 1 d . . .
H18 H 1.2519 0.9275 0.4858 0.027 Uiso 1 1 calc R . .
C19 C 1.16162(14) 0.85143(12) 0.29582(12) 0.0173(2) Uani 1 1 d . . .
C20 C 1.34540(14) 0.98069(11) 0.21534(12) 0.0171(2) Uani 1 1 d . . .
C21 C 1.38490(16) 1.05012(12) 0.14605(13) 0.0228(3) Uani 1 1 d . . .
H21 H 1.3349 1.0883 0.1070 0.027 Uiso 1 1 calc R . .
C22 C 1.49630(18) 1.06382(13) 0.13365(15) 0.0279(3) Uani 1 1 d . . .
H22 H 1.5230 1.1122 0.0873 0.033 Uiso 1 1 calc R . .
C23 C 1.56865(16) 1.00717(13) 0.18874(15) 0.0271(3) Uani 1 1 d . . .
H23 H 1.6449 1.0166 0.1802 0.032 Uiso 1 1 calc R . .
C24 C 1.52965(15) 0.93671(13) 0.25638(13) 0.0226(3) Uani 1 1 d . . .
H24 H 1.5786 0.8972 0.2936 0.027 Uiso 1 1 calc R . .
C25 C 1.41865(14) 0.92368(12) 0.26989(12) 0.0193(3) Uani 1 1 d . . .
H25 H 1.3927 0.8756 0.3167 0.023 Uiso 1 1 calc R . .
C26 C 1.30435(14) 1.11148(12) 0.36418(12) 0.0174(2) Uani 1 1 d . . .
C27 C 1.45004(15) 1.16342(12) 0.45965(13) 0.0206(3) Uani 1 1 d . . .
H27 H 1.4981 1.1238 0.4575 0.025 Uiso 1 1 calc R . .
C28 C 1.52592(16) 1.27286(12) 0.55826(13) 0.0227(3) Uani 1 1 d . . .
H28 H 1.6254 1.3078 0.6228 0.027 Uiso 1 1 calc R . .
C29 C 1.45616(17) 1.33097(13) 0.56227(14) 0.0240(3) Uani 1 1 d . . .
H29 H 1.5075 1.4051 0.6300 0.029 Uiso 1 1 calc R . .
C30 C 1.31189(17) 1.28090(13) 0.46764(14) 0.0246(3) Uani 1 1 d . . .
H30 H 1.2644 1.3209 0.4703 0.030 Uiso 1 1 calc R . .
C31 C 1.23606(15) 1.17188(13) 0.36843(14) 0.0215(3) Uani 1 1 d . . .
H31 H 1.1373 1.1384 0.3032 0.026 Uiso 1 1 calc R . .
C32 C 0.97569(14) 0.35723(12) 0.22370(12) 0.0193(3) Uani 1 1 d . . .
H32 H 0.9506 0.4201 0.2046 0.023 Uiso 1 1 calc R . .
Cl1 Cl 0.99075(4) 0.34333(4) 0.36401(3) 0.03069(9) Uani 1 1 d . . .
Cl2 Cl 0.83438(4) 0.21237(3) 0.10115(3) 0.02702(9) Uani 1 1 d . . .
Cl3 Cl 1.14339(4) 0.40819(4) 0.23914(4) 0.02798(9) 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
P1 C13 1.8212(13) . ?
P1 C1 1.8349(14) . ?
P1 C7 1.8366(14) . ?
P2 C19 1.8254(14) . ?
P2 C26 1.8345(14) . ?
P2 C20 1.8363(14) . ?
N1 C15 1.3319(17) . ?
N1 N2 1.3602(15) . ?
N2 C13 1.3659(16) . ?
N2 C16 1.4457(16) . ?
N3 N4 1.3564(16) . ?
N3 C19 1.3702(16) . ?
N3 C16 1.4544(17) . ?
N4 C17 1.3324(18) . ?
C1 C6 1.395(2) . ?
C1 C2 1.4008(18) . ?
C2 C3 1.393(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.3982(18) . ?
C7 C8 1.3999(19) . ?
C8 C9 1.387(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3905(19) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.3848(17) . ?
C14 C15 1.4044(18) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.405(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(2) . ?
C18 H18 0.9500 . ?
C20 C25 1.3950(19) . ?
C20 C21 1.3989(19) . ?
C21 C22 1.388(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.3942(19) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.3929(19) . ?
C26 C31 1.3981(19) . ?
C27 C28 1.3925(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.3934(19) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 Cl3 1.7606(14) . ?
C32 Cl2 1.7622(14) . ?
C32 Cl1 1.7702(14) . ?
C32 H32 1.0000 . ?

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
C13 P1 C1 101.33(6) . . ?
C13 P1 C7 97.32(6) . . ?
C1 P1 C7 102.49(6) . . ?
C19 P2 C26 100.09(6) . . ?
C19 P2 C20 100.69(6) . . ?
C26 P2 C20 101.21(6) . . ?
C15 N1 N2 104.27(10) . . ?
N1 N2 C13 112.78(10) . . ?
N1 N2 C16 118.45(10) . . ?
C13 N2 C16 128.71(11) . . ?
N4 N3 C19 113.10(11) . . ?
N4 N3 C16 119.53(10) . . ?
C19 N3 C16 127.14(11) . . ?
C17 N4 N3 103.98(11) . . ?
C6 C1 C2 118.70(13) . . ?
C6 C1 P1 123.77(10) . . ?
C2 C1 P1 117.53(11) . . ?
C3 C2 C1 120.27(14) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 120.43(14) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.78(14) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 120.06(14) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.74(13) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C12 C7 C8 118.94(12) . . ?
C12 C7 P1 123.60(10) . . ?
C8 C7 P1 117.45(10) . . ?
C9 C8 C7 120.52(13) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 120.06(13) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.79(13) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.35(13) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.32(13) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
N2 C13 C14 105.68(11) . . ?
N2 C13 P1 122.79(9) . . ?
C14 C13 P1 131.38(10) . . ?
C13 C14 C15 105.31(11) . . ?
C13 C14 H14 127.3 . . ?
C15 C14 H14 127.3 . . ?
N1 C15 C14 111.95(11) . . ?
N1 C15 H15 124.0 . . ?
C14 C15 H15 124.0 . . ?
N2 C16 N3 112.28(10) . . ?
N2 C16 H16A 109.1 . . ?
N3 C16 H16A 109.1 . . ?
N2 C16 H16B 109.1 . . ?
N3 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
N4 C17 C18 112.10(13) . . ?
N4 C17 H17 124.0 . . ?
C18 C17 H17 124.0 . . ?
C19 C18 C17 105.40(12) . . ?
C19 C18 H18 127.3 . . ?
C17 C18 H18 127.3 . . ?
N3 C19 C18 105.42(12) . . ?
N3 C19 P2 121.71(10) . . ?
C18 C19 P2 132.87(10) . . ?
C25 C20 C21 118.56(13) . . ?
C25 C20 P2 124.91(10) . . ?
C21 C20 P2 116.54(10) . . ?
C22 C21 C20 120.74(14) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C23 C22 C21 120.15(14) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 119.89(14) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 120.09(14) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 120.58(13) . . ?
C24 C25 H25 119.7 . . ?
C20 C25 H25 119.7 . . ?
C27 C26 C31 118.82(12) . . ?
C27 C26 P2 123.57(10) . . ?
C31 C26 P2 117.51(10) . . ?
C28 C27 C26 120.62(13) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 119.98(13) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.99(13) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.13(13) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C26 120.45(13) . . ?
C30 C31 H31 119.8 . . ?
C26 C31 H31 119.8 . . ?
Cl3 C32 Cl2 110.42(7) . . ?
Cl3 C32 Cl1 110.34(7) . . ?
Cl2 C32 Cl1 109.67(7) . . ?
Cl3 C32 H32 108.8 . . ?
Cl2 C32 H32 108.8 . . ?
Cl1 C32 H32 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_compound14_MSB686_0m_b
_database_code_depnum_ccdc_archive 'CCDC 1511155'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H50 N4 P2 Rh2, 2(B F4)'
_chemical_formula_sum            'C47 H50 B2 F8 N4 P2 Rh2'
_chemical_formula_weight         1112.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.8580(3)
_cell_length_b                   11.7581(3)
_cell_length_c                   13.3446(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.8490(6)
_cell_angle_gamma                90
_cell_volume                     2354.80(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      3.500
_cell_measurement_theta_max      72.189

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             1124
_exptl_transmission_factor_min   0.453
_exptl_transmission_factor_max   0.757
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    6.912
_shelx_estimated_absorpt_T_min   0.467
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_T_max  0.82

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            17112
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.500
_diffrn_reflns_theta_max         72.182
_diffrn_reflns_theta_full        68.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             4256
_reflns_number_gt                4209
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_max     0.862
_reflns_Friedel_fraction_full    0.925

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

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT  (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Bruker AXS 2013c)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.99 Å) except for the olefinic 
ones in the cyclooctadiene ligand which were located in a difference map 
and their coordinateds adjusted to give C---H = 0.98 Å. All were included 
as riding contributions with isotropic displacement parameters 1.2 - 1.5 
times those of the attached carbon atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0218P)²+3.9606P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1854 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack, 2004).
;
_refine_ls_abs_structure_Flack   0.027(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4256
_refine_ls_number_parameters     294
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.062
_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
Rh1 Rh 0.56538(2) 0.11042(4) -0.20019(2) 0.01448(9) Uani 1 1 d . U . . .
P1 P 0.55206(7) -0.01260(8) 0.21057(8) 0.0160(2) Uani 1 1 d . U . . .
N1 N 0.5779(2) 0.0784(2) 0.0292(2) 0.0139(7) Uani 1 1 d . U . . .
N2 N 0.6255(2) 0.0687(3) -0.0379(3) 0.0160(7) Uani 1 1 d . U . . .
C1 C 0.6454(3) -0.0302(4) 0.3333(3) 0.0202(8) Uani 1 1 d . U . . .
C2 C 0.7148(3) 0.0484(4) 0.3605(4) 0.0266(10) Uani 1 1 d . U . . .
H2 H 0.7144 0.1106 0.3150 0.032 Uiso 1 1 calc R U . . .
C3 C 0.7849(3) 0.0351(5) 0.4552(4) 0.0357(12) Uani 1 1 d . U . . .
H3 H 0.8329 0.0878 0.4733 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7851(3) -0.0539(5) 0.5226(4) 0.0361(12) Uani 1 1 d . U . . .
H4 H 0.8328 -0.0618 0.5872 0.043 Uiso 1 1 calc R U . . .
C5 C 0.7158(4) -0.1316(5) 0.4964(4) 0.0345(11) Uani 1 1 d . U . . .
H5 H 0.7158 -0.1925 0.5432 0.041 Uiso 1 1 calc R U . . .
C6 C 0.6463(3) -0.1206(4) 0.4019(3) 0.0265(10) Uani 1 1 d . U . . .
H6 H 0.5992 -0.1746 0.3836 0.032 Uiso 1 1 calc R U . . .
C7 C 0.5095(3) -0.1568(4) 0.1760(3) 0.0212(8) Uani 1 1 d . U . . .
C8 C 0.5612(3) -0.2430(4) 0.1538(4) 0.0296(10) Uani 1 1 d . U . . .
H8 H 0.6203 -0.2271 0.1549 0.035 Uiso 1 1 calc R U . . .
C9 C 0.5269(4) -0.3519(4) 0.1300(4) 0.0373(12) Uani 1 1 d . U . . .
H9 H 0.5626 -0.4109 0.1164 0.045 Uiso 1 1 calc R U . . .
C10 C 0.4393(4) -0.3740(5) 0.1263(4) 0.0403(13) Uani 1 1 d . U . . .
H10 H 0.4149 -0.4479 0.1079 0.048 Uiso 1 1 calc R U . . .
C11 C 0.3882(4) -0.2896(4) 0.1492(5) 0.0397(13) Uani 1 1 d . U . . .
H11 H 0.3290 -0.3056 0.1477 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4233(3) -0.1807(4) 0.1747(4) 0.0281(10) Uani 1 1 d . U . . .
H12 H 0.3882 -0.1227 0.1913 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6131(3) 0.0146(3) 0.1179(3) 0.0178(8) Uani 1 1 d . U . . .
C14 C 0.6891(3) -0.0341(4) 0.1090(4) 0.0254(11) Uani 1 1 d . U . . .
H14 H 0.7298 -0.0819 0.1593 0.031 Uiso 1 1 calc R U . . .
C15 C 0.6944(3) 0.0009(4) 0.0107(3) 0.0198(8) Uani 1 1 d . U . . .
H15 H 0.7401 -0.0204 -0.0173 0.024 Uiso 1 1 calc R U . . .
C16 C 0.5000 0.1492(5) 0.0000 0.0151(11) Uani 1 2 d S TU P . .
H16A H 0.5004 0.1985 0.0603 0.018 Uiso 0.5 1 calc R U P . .
H16B H 0.4996 0.1985 -0.0603 0.018 Uiso 0.5 1 calc R U P . .
C17 C 0.6938(3) 0.1853(4) -0.2029(3) 0.0188(8) Uani 1 1 d . U . . .
H17 H 0.7361 0.1441 -0.1441 0.023 Uiso 1 1 d R U . . .
C18 C 0.6429(3) 0.2692(4) -0.1784(3) 0.0217(9) Uani 1 1 d . U . . .
H18 H 0.6537 0.2870 -0.1035 0.026 Uiso 1 1 d R U . . .
C19 C 0.5855(3) 0.3563(4) -0.2519(4) 0.0286(10) Uani 1 1 d . U . . .
H19A H 0.6240 0.4182 -0.2626 0.034 Uiso 1 1 calc R U . . .
H19B H 0.5441 0.3897 -0.2182 0.034 Uiso 1 1 calc R U . . .
C20 C 0.5318(3) 0.3077(4) -0.3592(4) 0.0290(10) Uani 1 1 d . U . . .
H20A H 0.4798 0.3575 -0.3921 0.035 Uiso 1 1 calc R U . . .
H20B H 0.5692 0.3073 -0.4060 0.035 Uiso 1 1 calc R U . . .
C21 C 0.4992(3) 0.1878(4) -0.3510(3) 0.0204(9) Uani 1 1 d . U . . .
H21 H 0.4352 0.1808 -0.3626 0.024 Uiso 1 1 d R U . . .
C22 C 0.5443(3) 0.0905(4) -0.3649(3) 0.0219(11) Uani 1 1 d . U . . .
H22 H 0.5096 0.0204 -0.3849 0.026 Uiso 1 1 d R U . . .
C23 C 0.6356(3) 0.0833(4) -0.3791(3) 0.0271(12) Uani 1 1 d . U . . .
H23A H 0.6287 0.0969 -0.4546 0.033 Uiso 1 1 calc R U . . .
H23B H 0.6591 0.0053 -0.3613 0.033 Uiso 1 1 calc R U . . .
C24 C 0.7035(3) 0.1676(4) -0.3116(3) 0.0240(9) Uani 1 1 d . U . . .
H24A H 0.7643 0.1395 -0.3029 0.029 Uiso 1 1 calc R U . . .
H24B H 0.6961 0.2416 -0.3489 0.029 Uiso 1 1 calc R U . . .
B1 B 0.6704(4) 0.3511(5) 0.1697(5) 0.0335(13) Uani 1 1 d . U . . .
F1 F 0.5979(4) 0.3374(7) 0.1947(6) 0.132(3) Uani 1 1 d . U . . .
F2 F 0.7426(5) 0.3003(5) 0.2541(3) 0.1010(18) Uani 1 1 d . U . . .
F3 F 0.6987(3) 0.4590(3) 0.1691(3) 0.0614(10) Uani 1 1 d . U . . .
F4 F 0.6721(3) 0.2950(4) 0.0799(3) 0.0657(12) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N2 2.123(3) . ?
Rh1 C22 2.126(4) . ?
Rh1 C21 2.148(4) . ?
Rh1 C18 2.202(4) . ?
Rh1 C17 2.229(4) . ?
Rh1 P1 2.3265(10) 2_655 ?
P1 C13 1.828(4) . ?
P1 C7 1.828(4) . ?
P1 C1 1.830(4) . ?
P1 Rh1 2.3265(10) 2_655 ?
N1 N2 1.350(5) . ?
N1 C13 1.359(5) . ?
N1 C16 1.436(4) . ?
N2 C15 1.338(5) . ?
C1 C2 1.392(7) . ?
C1 C6 1.400(6) . ?
C2 C3 1.396(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.390(6) . ?
C7 C8 1.395(6) . ?
C8 C9 1.387(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.373(6) . ?
C14 C15 1.404(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 N1 1.436(4) 2_655 ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.380(6) . ?
C17 C24 1.523(6) . ?
C17 H17 0.9800 . ?
C18 C19 1.504(6) . ?
C18 H18 0.9800 . ?
C19 C20 1.521(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.518(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.392(6) . ?
C21 H21 0.9800 . ?
C22 C23 1.522(6) . ?
C22 H22 0.9800 . ?
C23 C24 1.526(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
B1 F1 1.307(7) . ?
B1 F3 1.346(7) . ?
B1 F4 1.375(7) . ?
B1 F2 1.450(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Rh1 C22 153.87(15) . . ?
N2 Rh1 C21 167.47(15) . . ?
C22 Rh1 C21 38.02(17) . . ?
N2 Rh1 C18 90.76(15) . . ?
C22 Rh1 C18 97.16(18) . . ?
C21 Rh1 C18 81.23(16) . . ?
N2 Rh1 C17 89.75(14) . . ?
C22 Rh1 C17 82.32(16) . . ?
C21 Rh1 C17 89.42(16) . . ?
C18 Rh1 C17 36.27(16) . . ?
N2 Rh1 P1 90.25(9) . 2_655 ?
C22 Rh1 P1 90.84(13) . 2_655 ?
C21 Rh1 P1 93.92(12) . 2_655 ?
C18 Rh1 P1 159.51(12) . 2_655 ?
C17 Rh1 P1 164.21(11) . 2_655 ?
C13 P1 C7 102.97(19) . . ?
C13 P1 C1 99.97(19) . . ?
C7 P1 C1 104.3(2) . . ?
C13 P1 Rh1 116.07(14) . 2_655 ?
C7 P1 Rh1 109.77(15) . 2_655 ?
C1 P1 Rh1 121.59(14) . 2_655 ?
N2 N1 C13 111.8(3) . . ?
N2 N1 C16 119.1(3) . . ?
C13 N1 C16 129.1(3) . . ?
C15 N2 N1 105.8(3) . . ?
C15 N2 Rh1 131.2(3) . . ?
N1 N2 Rh1 119.6(2) . . ?
C2 C1 C6 119.6(4) . . ?
C2 C1 P1 120.1(3) . . ?
C6 C1 P1 120.3(4) . . ?
C1 C2 C3 119.5(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.1(5) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C12 C7 C8 119.6(4) . . ?
C12 C7 P1 118.2(4) . . ?
C8 C7 P1 122.2(4) . . ?
C9 C8 C7 120.3(5) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.5(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.5(5) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C7 C12 C11 120.1(5) . . ?
C7 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
N1 C13 C14 106.2(4) . . ?
N1 C13 P1 121.9(3) . . ?
C14 C13 P1 131.0(3) . . ?
C13 C14 C15 106.1(4) . . ?
C13 C14 H14 126.9 . . ?
C15 C14 H14 126.9 . . ?
N2 C15 C14 110.0(4) . . ?
N2 C15 H15 125.0 . . ?
C14 C15 H15 125.0 . . ?
N1 C16 N1 109.2(4) 2_655 . ?
N1 C16 H16A 109.9 2_655 . ?
N1 C16 H16A 109.9 . . ?
N1 C16 H16B 109.9 2_655 . ?
N1 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C18 C17 C24 124.8(4) . . ?
C18 C17 Rh1 70.8(2) . . ?
C24 C17 Rh1 109.6(3) . . ?
C18 C17 H17 117.8 . . ?
C24 C17 H17 116.2 . . ?
Rh1 C17 H17 100.7 . . ?
C17 C18 C19 127.5(4) . . ?
C17 C18 Rh1 72.9(2) . . ?
C19 C18 Rh1 107.3(3) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 H18 112.9 . . ?
Rh1 C18 H18 102.9 . . ?
C18 C19 C20 113.3(4) . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 112.4(4) . . ?
C21 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C20 123.5(4) . . ?
C22 C21 Rh1 70.1(2) . . ?
C20 C21 Rh1 112.8(3) . . ?
C22 C21 H21 117.4 . . ?
C20 C21 H21 115.3 . . ?
Rh1 C21 H21 106.2 . . ?
C21 C22 C23 127.8(4) . . ?
C21 C22 Rh1 71.8(2) . . ?
C23 C22 Rh1 107.3(3) . . ?
C21 C22 H22 117.4 . . ?
C23 C22 H22 113.1 . . ?
Rh1 C22 H22 105.1 . . ?
C22 C23 C24 114.1(4) . . ?
C22 C23 H23A 108.7 . . ?
C24 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
C24 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C17 C24 C23 112.5(3) . . ?
C17 C24 H24A 109.1 . . ?
C23 C24 H24A 109.1 . . ?
C17 C24 H24B 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
F1 B1 F3 116.1(6) . . ?
F1 B1 F4 115.4(5) . . ?
F3 B1 F4 110.3(5) . . ?
F1 B1 F2 106.8(6) . . ?
F3 B1 F2 102.2(5) . . ?
F4 B1 F2 104.3(5) . . ?

_refine_diff_density_max         0.898
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_compound16_MSB589_0m
_database_code_depnum_ccdc_archive 'CCDC 1511156'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 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         'C31 H26 Cl2 N4 P2 Pd'
_chemical_formula_sum            'C31 H26 Cl2 N4 P2 Pd'
_chemical_formula_weight         693.80

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'
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'
Pd Pd -0.9988 1.0072 '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                   12.041(4)
_cell_length_b                   18.039(6)
_cell_length_c                   13.169(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.438(4)
_cell_angle_gamma                90
_cell_volume                     2857.8(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.36

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   0.792
_exptl_transmission_factor_max   0.976
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    0.978
_shelx_estimated_absorpt_T_min   0.859
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 The diffraction data were collected in three sets of
 606 frames (0.3 deg. width in omega) at phi = 0, 120
 and 240 deg. A scan time of 40 sec/frame was used. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24568
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.693
_diffrn_reflns_theta_max         28.530
_diffrn_reflns_theta_full        27.300
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6702
_reflns_number_gt                5772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2008)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'

_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. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0517P)²+3.2961P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6702
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_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
Pd1 Pd 0.28841(2) 0.46370(2) 0.86688(2) 0.01451(7) Uani 1 1 d . . . . .
Cl1 Cl 0.40321(6) 0.35764(4) 0.87235(5) 0.02479(15) Uani 1 1 d . . . . .
Cl2 Cl 0.21323(5) 0.43474(4) 1.02253(5) 0.01971(14) Uani 1 1 d . . . . .
P1 P 0.22550(5) 0.58076(4) 0.87321(5) 0.01440(14) Uani 1 1 d . . . . .
P2 P 0.34032(6) 0.47410(4) 0.70484(5) 0.01615(14) Uani 1 1 d . . . . .
N1 N 0.44881(18) 0.63039(13) 0.85237(17) 0.0190(5) Uani 1 1 d . . . . .
N2 N 0.3176(2) 0.71650(13) 0.83148(19) 0.0243(5) Uani 1 1 d . . . . .
N3 N 0.54721(19) 0.52893(13) 0.77703(17) 0.0185(5) Uani 1 1 d . . . . .
N4 N 0.5509(2) 0.46946(14) 0.62886(18) 0.0239(5) Uani 1 1 d . . . . .
C1 C 0.1070(2) 0.59708(15) 0.78791(19) 0.0166(5) Uani 1 1 d . . . . .
C2 C 0.0829(2) 0.66418(15) 0.7382(2) 0.0210(6) Uani 1 1 d . . . . .
H2 H 0.1323 0.7051 0.7456 0.025 Uiso 1 1 calc R U . . .
C3 C -0.0140(3) 0.66987(16) 0.6781(2) 0.0261(6) Uani 1 1 d . . . . .
H3 H -0.0302 0.7150 0.6433 0.031 Uiso 1 1 calc R U . . .
C4 C -0.0874(2) 0.61143(17) 0.6678(2) 0.0255(6) Uani 1 1 d . . . . .
H4 H -0.1536 0.6165 0.6266 0.031 Uiso 1 1 calc R U . . .
C5 C -0.0644(2) 0.54494(16) 0.7180(2) 0.0236(6) Uani 1 1 d . . . . .
H5 H -0.1148 0.5046 0.7112 0.028 Uiso 1 1 calc R U . . .
C6 C 0.0327(2) 0.53789(15) 0.7779(2) 0.0196(5) Uani 1 1 d . . . . .
H6 H 0.0486 0.4926 0.8122 0.023 Uiso 1 1 calc R U . . .
C7 C 0.1828(2) 0.61085(14) 0.99691(19) 0.0177(5) Uani 1 1 d . . . . .
C8 C 0.0701(2) 0.61784(15) 1.0158(2) 0.0220(6) Uani 1 1 d . . . . .
H8 H 0.0154 0.6103 0.9626 0.026 Uiso 1 1 calc R U . . .
C9 C 0.0385(3) 0.63587(16) 1.1130(2) 0.0281(7) Uani 1 1 d . . . . .
H9 H -0.0381 0.6412 1.1260 0.034 Uiso 1 1 calc R U . . .
C10 C 0.1169(3) 0.64607(16) 1.1903(2) 0.0294(7) Uani 1 1 d . . . . .
H10 H 0.0944 0.6578 1.2567 0.035 Uiso 1 1 calc R U . . .
C11 C 0.2294(3) 0.63921(17) 1.1716(2) 0.0322(7) Uani 1 1 d . . . . .
H11 H 0.2837 0.6465 1.2251 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2623(3) 0.62179(16) 1.0748(2) 0.0247(6) Uani 1 1 d . . . . .
H12 H 0.3391 0.6174 1.0619 0.030 Uiso 1 1 calc R U . . .
C13 C 0.3365(2) 0.64547(15) 0.8479(2) 0.0177(5) Uani 1 1 d . . . . .
C14 C 0.5018(3) 0.69660(17) 0.8362(2) 0.0275(6) Uani 1 1 d . . . . .
H14 H 0.5796 0.7046 0.8342 0.033 Uiso 1 1 calc R U . . .
C15 C 0.4207(3) 0.74820(17) 0.8237(3) 0.0296(7) Uani 1 1 d . . . . .
H15 H 0.4333 0.7993 0.8113 0.036 Uiso 1 1 calc R U . . .
C16 C 0.2864(2) 0.54697(15) 0.6205(2) 0.0185(5) Uani 1 1 d . . . . .
C17 C 0.3461(3) 0.61253(16) 0.6067(2) 0.0233(6) Uani 1 1 d . . . . .
H17 H 0.4162 0.6194 0.6414 0.028 Uiso 1 1 calc R U . . .
C18 C 0.3039(3) 0.66682(17) 0.5434(2) 0.0278(6) Uani 1 1 d . . . . .
H18 H 0.3452 0.7110 0.5343 0.033 Uiso 1 1 calc R U . . .
C19 C 0.2014(3) 0.65793(18) 0.4922(2) 0.0305(7) Uani 1 1 d . . . . .
H19 H 0.1727 0.6960 0.4488 0.037 Uiso 1 1 calc R U . . .
C20 C 0.1411(3) 0.59339(17) 0.5047(2) 0.0275(6) Uani 1 1 d . . . . .
H20 H 0.0710 0.5871 0.4699 0.033 Uiso 1 1 calc R U . . .
C21 C 0.1842(2) 0.53757(16) 0.5688(2) 0.0221(6) Uani 1 1 d . . . . .
H21 H 0.1434 0.4930 0.5771 0.027 Uiso 1 1 calc R U . . .
C22 C 0.3056(2) 0.38998(15) 0.6349(2) 0.0198(5) Uani 1 1 d . . . . .
C23 C 0.2205(3) 0.34512(18) 0.6682(2) 0.0313(7) Uani 1 1 d . . . . .
H23 H 0.1849 0.3569 0.7292 0.038 Uiso 1 1 calc R U . . .
C24 C 0.1875(3) 0.28280(19) 0.6120(3) 0.0364(8) Uani 1 1 d . . . . .
H24 H 0.1290 0.2523 0.6341 0.044 Uiso 1 1 calc R U . . .
C25 C 0.2405(3) 0.26555(17) 0.5239(2) 0.0318(7) Uani 1 1 d . . . . .
H25 H 0.2187 0.2228 0.4859 0.038 Uiso 1 1 calc R U . . .
C26 C 0.3251(3) 0.31032(17) 0.4909(2) 0.0292(7) Uani 1 1 d . . . . .
H26 H 0.3614 0.2979 0.4305 0.035 Uiso 1 1 calc R U . . .
C27 C 0.3573(2) 0.37296(16) 0.5452(2) 0.0241(6) Uani 1 1 d . . . . .
H27 H 0.4142 0.4041 0.5215 0.029 Uiso 1 1 calc R U . . .
C28 C 0.4878(2) 0.48873(15) 0.7041(2) 0.0190(5) Uani 1 1 d . . . . .
C29 C 0.6532(2) 0.53486(18) 0.7440(2) 0.0253(6) Uani 1 1 d . . . . .
H29 H 0.7140 0.5596 0.7775 0.030 Uiso 1 1 calc R U . . .
C30 C 0.6541(2) 0.49832(19) 0.6541(2) 0.0271(6) Uani 1 1 d . . . . .
H30 H 0.7174 0.4933 0.6140 0.033 Uiso 1 1 calc R U . . .
C31 C 0.5098(2) 0.56179(16) 0.8708(2) 0.0194(5) Uani 1 1 d . . . . .
H31A H 0.4615 0.5260 0.9050 0.023 Uiso 1 1 calc R U . . .
H31B H 0.5751 0.5719 0.9169 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 P1 2.2461(9) . ?
Pd1 P2 2.2568(9) . ?
Pd1 Cl2 2.3350(9) . ?
Pd1 Cl1 2.3597(9) . ?
P1 C1 1.803(3) . ?
P1 C7 1.812(3) . ?
P1 C13 1.817(3) . ?
P2 C28 1.796(3) . ?
P2 C22 1.814(3) . ?
P2 C16 1.822(3) . ?
N1 C14 1.375(4) . ?
N1 C13 1.378(3) . ?
N1 C31 1.454(4) . ?
N2 C13 1.318(4) . ?
N2 C15 1.374(4) . ?
N3 C29 1.369(4) . ?
N3 C28 1.379(4) . ?
N3 C31 1.458(3) . ?
N4 C28 1.320(4) . ?
N4 C30 1.376(4) . ?
C1 C6 1.396(4) . ?
C1 C2 1.400(4) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.388(4) . ?
C7 C8 1.396(4) . ?
C8 C9 1.389(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.354(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.391(4) . ?
C16 C17 1.400(4) . ?
C17 C18 1.370(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.400(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.391(4) . ?
C22 C27 1.393(4) . ?
C23 C24 1.394(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C29 C30 1.356(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Pd1 P2 93.69(2) . . ?
P1 Pd1 Cl2 91.94(3) . . ?
P2 Pd1 Cl2 169.11(3) . . ?
P1 Pd1 Cl1 163.57(3) . . ?
P2 Pd1 Cl1 84.88(3) . . ?
Cl2 Pd1 Cl1 92.31(3) . . ?
C1 P1 C7 105.31(12) . . ?
C1 P1 C13 110.49(13) . . ?
C7 P1 C13 102.23(12) . . ?
C1 P1 Pd1 112.93(9) . . ?
C7 P1 Pd1 115.09(9) . . ?
C13 P1 Pd1 110.20(9) . . ?
C28 P2 C22 109.09(13) . . ?
C28 P2 C16 102.58(13) . . ?
C22 P2 C16 103.03(13) . . ?
C28 P2 Pd1 109.32(9) . . ?
C22 P2 Pd1 110.06(9) . . ?
C16 P2 Pd1 122.01(9) . . ?
C14 N1 C13 106.4(2) . . ?
C14 N1 C31 122.1(2) . . ?
C13 N1 C31 131.5(2) . . ?
C13 N2 C15 105.5(2) . . ?
C29 N3 C28 106.4(2) . . ?
C29 N3 C31 124.2(2) . . ?
C28 N3 C31 129.3(2) . . ?
C28 N4 C30 105.2(2) . . ?
C6 C1 C2 119.9(3) . . ?
C6 C1 P1 114.9(2) . . ?
C2 C1 P1 125.1(2) . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C12 C7 C8 120.1(3) . . ?
C12 C7 P1 119.6(2) . . ?
C8 C7 P1 120.2(2) . . ?
C9 C8 C7 119.4(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C7 119.8(3) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
N2 C13 N1 111.2(2) . . ?
N2 C13 P1 122.1(2) . . ?
N1 C13 P1 126.4(2) . . ?
C15 C14 N1 106.2(3) . . ?
C15 C14 H14 126.9 . . ?
N1 C14 H14 126.9 . . ?
C14 C15 N2 110.7(3) . . ?
C14 C15 H15 124.6 . . ?
N2 C15 H15 124.6 . . ?
C21 C16 C17 119.2(3) . . ?
C21 C16 P2 119.7(2) . . ?
C17 C16 P2 121.1(2) . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C20 C19 C18 119.9(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C16 C21 C20 120.3(3) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C27 120.1(3) . . ?
C23 C22 P2 118.9(2) . . ?
C27 C22 P2 120.8(2) . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C22 119.6(3) . . ?
C26 C27 H27 120.2 . . ?
C22 C27 H27 120.2 . . ?
N4 C28 N3 111.3(2) . . ?
N4 C28 P2 124.4(2) . . ?
N3 C28 P2 123.9(2) . . ?
C30 C29 N3 106.4(3) . . ?
C30 C29 H29 126.8 . . ?
N3 C29 H29 126.8 . . ?
C29 C30 N4 110.7(3) . . ?
C29 C30 H30 124.6 . . ?
N4 C30 H30 124.6 . . ?
N1 C31 N3 112.1(2) . . ?
N1 C31 H31A 109.2 . . ?
N3 C31 H31A 109.2 . . ?
N1 C31 H31B 109.2 . . ?
N3 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?

_refine_diff_density_max         1.486
_refine_diff_density_min         -0.995
_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_compound18_msb663_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1511157'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
cis-Dichlorido(5-(diphenylphosphanyl)-1-{[5-diphenylphosphanyl-1H-1,2,4-triazol-1-yl]methyl}-1H-1,2,4-triazole-κ²P,P')palladium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H24 Cl2 N6 P2 Pd'
_chemical_formula_sum            'C29 H24 Cl2 N6 P2 Pd'
_chemical_formula_weight         695.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.9501(3)
_cell_length_b                   24.6633(9)
_cell_length_c                   11.4922(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.4310(16)
_cell_angle_gamma                90
_cell_volume                     2789.73(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9845
_cell_measurement_theta_min      3.5842
_cell_measurement_theta_max      72.5478

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   0.490
_exptl_transmission_factor_max   0.806
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    8.474
_shelx_estimated_absorpt_T_min   0.282
_shelx_estimated_absorpt_T_max   0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2013b)'
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_T_max  0.79

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            10351
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.584
_diffrn_reflns_theta_max         72.539
_diffrn_reflns_theta_full        70.500
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5425
_reflns_number_gt                4324
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. H-atoms were placed in
calculated positions (C---H = 0.95 Å) and included as riding
contributions with isotropic displacement parameters 1.2 times those
of the attached carbon atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+3.1654P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5425
_refine_ls_number_parameters     361
_refine_ls_number_restraints     345
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0726
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.003
_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
Pd1 Pd 0.00040(2) 0.60597(2) 0.99710(2) 0.01041(7) Uani 1 1 d . U . . .
Cl1 Cl -0.10483(8) 0.60912(3) 1.16713(7) 0.01611(17) Uani 1 1 d . U . . .
Cl2 Cl -0.18927(8) 0.56405(3) 0.89527(7) 0.01740(17) Uani 1 1 d . U . . .
P1 P 0.17372(8) 0.64608(3) 1.11688(7) 0.01096(17) Uani 1 1 d . U . . .
P2 P 0.09052(8) 0.62107(3) 0.83086(7) 0.01086(17) Uani 1 1 d . U . . .
N1 N 0.1384(3) 0.73694(11) 1.2591(3) 0.0179(6) Uani 1 1 d . U . . .
N2 N 0.0000(3) 0.78994(10) 1.1323(3) 0.0181(6) Uani 1 1 d . U . . .
N3 N 0.0217(3) 0.74132(10) 1.0815(2) 0.0139(6) Uani 1 1 d . U . . .
N4 N 0.0635(3) 0.73338(10) 0.8810(2) 0.0128(6) Uani 1 1 d . U . . .
N5 N 0.1142(3) 0.78286(10) 0.8574(2) 0.0150(6) Uani 1 1 d . U . . .
N6 N 0.2174(3) 0.71624(10) 0.7676(2) 0.0152(6) Uani 1 1 d . U . . .
C1 C 0.2331(3) 0.60683(12) 1.2482(3) 0.0128(6) Uani 1 1 d . U . . .
C2 C 0.1908(3) 0.55366(13) 1.2567(3) 0.0158(7) Uani 1 1 d . U . . .
H2 H 0.1262 0.5384 1.1965 0.019 Uiso 1 1 calc R U . . .
C3 C 0.2434(3) 0.52282(13) 1.3538(3) 0.0175(7) Uani 1 1 d . U . . .
H3 H 0.2155 0.4862 1.3594 0.021 Uiso 1 1 calc R U . . .
C4 C 0.3357(3) 0.54489(13) 1.4422(3) 0.0190(7) Uani 1 1 d . U . . .
H4 H 0.3692 0.5238 1.5095 0.023 Uiso 1 1 calc R U . . .
C5 C 0.3800(4) 0.59808(14) 1.4330(3) 0.0245(8) Uani 1 1 d . U . . .
H5 H 0.4439 0.6134 1.4937 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3306(4) 0.62845(14) 1.3350(3) 0.0210(8) Uani 1 1 d . U . . .
H6 H 0.3632 0.6642 1.3268 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3320(3) 0.66990(12) 1.0725(3) 0.0113(6) Uani 1 1 d . U . . .
C8 C 0.4329(3) 0.63203(13) 1.0594(3) 0.0149(7) Uani 1 1 d . U . . .
H8 H 0.4159 0.5944 1.0681 0.018 Uiso 1 1 calc R U . . .
C9 C 0.5581(3) 0.64938(13) 1.0337(3) 0.0169(7) Uani 1 1 d . U . . .
H9 H 0.6268 0.6236 1.0245 0.020 Uiso 1 1 calc R U . . .
C10 C 0.5829(3) 0.70402(14) 1.0216(3) 0.0177(7) Uani 1 1 d . U . . .
H10 H 0.6693 0.7157 1.0054 0.021 Uiso 1 1 calc R U . . .
C11 C 0.4832(3) 0.74203(14) 1.0327(3) 0.0181(7) Uani 1 1 d . U . . .
H11 H 0.5005 0.7795 1.0229 0.022 Uiso 1 1 calc R U . . .
C12 C 0.3579(3) 0.72511(13) 1.0583(3) 0.0149(7) Uani 1 1 d . U . . .
H12 H 0.2894 0.7511 1.0662 0.018 Uiso 1 1 calc R U . . .
C13 C 0.1049(3) 0.71014(12) 1.1589(3) 0.0129(6) Uani 1 1 d . U . . .
C14 C 0.0703(4) 0.78486(13) 1.2376(3) 0.0207(8) Uani 1 1 d . U . . .
H14 H 0.0737 0.8127 1.2952 0.025 Uiso 1 1 calc R U . . .
C15 C -0.0385(3) 0.73184(13) 0.9601(3) 0.0150(7) Uani 1 1 d . U . . .
H15A H -0.1084 0.7598 0.9359 0.018 Uiso 1 1 calc R U . . .
H15B H -0.0839 0.6960 0.9540 0.018 Uiso 1 1 calc R U . . .
C16 C 0.2063(3) 0.76990(13) 0.7905(3) 0.0172(7) Uani 1 1 d . U . . .
H16 H 0.2613 0.7964 0.7603 0.021 Uiso 1 1 calc R U . . .
C17 C 0.1274(3) 0.69384(12) 0.8272(3) 0.0124(6) Uani 1 1 d . U . . .
C18 C -0.0141(3) 0.61216(12) 0.6887(3) 0.0122(6) Uani 1 1 d . U . . .
C19 C -0.1428(3) 0.63603(12) 0.6682(3) 0.0158(7) Uani 1 1 d . U . . .
H19 H -0.1758 0.6556 0.7293 0.019 Uiso 1 1 calc R U . . .
C20 C -0.2224(3) 0.63127(13) 0.5593(3) 0.0175(7) Uani 1 1 d . U . . .
H20 H -0.3101 0.6473 0.5463 0.021 Uiso 1 1 calc R U . . .
C21 C -0.1744(4) 0.60316(14) 0.4688(3) 0.0208(7) Uani 1 1 d . U . . .
H21 H -0.2286 0.6003 0.3938 0.025 Uiso 1 1 calc R U . . .
C22 C -0.0475(4) 0.57949(15) 0.4886(3) 0.0243(8) Uani 1 1 d . U . . .
H22 H -0.0144 0.5604 0.4268 0.029 Uiso 1 1 calc R U . . .
C23 C 0.0324(3) 0.58331(14) 0.5983(3) 0.0180(7) Uani 1 1 d . U . . .
H23 H 0.1189 0.5662 0.6115 0.022 Uiso 1 1 calc R U . . .
C24 C 0.2459(3) 0.58422(13) 0.8221(3) 0.0124(6) Uani 1 1 d . U . . .
C25 C 0.2548(3) 0.53319(13) 0.8756(3) 0.0189(7) Uani 1 1 d . U . . .
H25 H 0.1848 0.5209 0.9171 0.023 Uiso 1 1 calc R U . . .
C26 C 0.3663(3) 0.50072(14) 0.8676(3) 0.0239(8) Uani 1 1 d . U . . .
H26 H 0.3724 0.4658 0.9030 0.029 Uiso 1 1 calc R U . . .
C27 C 0.4690(3) 0.51875(14) 0.8085(3) 0.0208(8) Uani 1 1 d . U . . .
H27 H 0.5459 0.4964 0.8042 0.025 Uiso 1 1 calc R U . . .
C28 C 0.4600(3) 0.56946(13) 0.7553(3) 0.0170(7) Uani 1 1 d . U . . .
H28 H 0.5311 0.5817 0.7151 0.020 Uiso 1 1 calc R U . . .
C29 C 0.3483(3) 0.60217(13) 0.7604(3) 0.0159(7) Uani 1 1 d . U . . .
H29 H 0.3413 0.6365 0.7223 0.019 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 P2 2.2572(9) . ?
Pd1 P1 2.2696(8) . ?
Pd1 Cl2 2.3136(8) . ?
Pd1 Cl1 2.3495(8) . ?
P1 C13 1.816(3) . ?
P1 C1 1.817(3) . ?
P1 C7 1.822(3) . ?
P2 C24 1.809(3) . ?
P2 C18 1.817(3) . ?
P2 C17 1.834(3) . ?
N1 C13 1.327(4) . ?
N1 C14 1.366(4) . ?
N2 C14 1.312(5) . ?
N2 N3 1.365(4) . ?
N3 C13 1.361(4) . ?
N3 C15 1.454(4) . ?
N4 C17 1.362(4) . ?
N4 N5 1.363(3) . ?
N4 C15 1.459(4) . ?
N5 C16 1.319(4) . ?
N6 C17 1.325(4) . ?
N6 C16 1.357(4) . ?
C1 C2 1.385(4) . ?
C1 C6 1.392(5) . ?
C2 C3 1.388(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.395(4) . ?
C7 C12 1.400(4) . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16 0.9500 . ?
C18 C23 1.393(5) . ?
C18 C19 1.398(4) . ?
C19 C20 1.384(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.397(4) . ?
C24 C25 1.398(4) . ?
C25 C26 1.382(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

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
P2 Pd1 P1 94.62(3) . . ?
P2 Pd1 Cl2 92.37(3) . . ?
P1 Pd1 Cl2 172.97(3) . . ?
P2 Pd1 Cl1 168.30(3) . . ?
P1 Pd1 Cl1 82.70(3) . . ?
Cl2 Pd1 Cl1 90.31(3) . . ?
C13 P1 C1 109.38(15) . . ?
C13 P1 C7 99.74(14) . . ?
C1 P1 C7 102.42(15) . . ?
C13 P1 Pd1 104.94(11) . . ?
C1 P1 Pd1 113.39(11) . . ?
C7 P1 Pd1 125.59(10) . . ?
C24 P2 C18 105.71(15) . . ?
C24 P2 C17 108.35(15) . . ?
C18 P2 C17 100.83(14) . . ?
C24 P2 Pd1 114.38(11) . . ?
C18 P2 Pd1 119.67(11) . . ?
C17 P2 Pd1 106.67(11) . . ?
C13 N1 C14 102.7(3) . . ?
C14 N2 N3 102.4(3) . . ?
C13 N3 N2 109.6(3) . . ?
C13 N3 C15 131.4(3) . . ?
N2 N3 C15 118.9(3) . . ?
C17 N4 N5 109.8(3) . . ?
C17 N4 C15 132.7(3) . . ?
N5 N4 C15 117.4(2) . . ?
C16 N5 N4 102.0(3) . . ?
C17 N6 C16 103.1(3) . . ?
C2 C1 C6 120.0(3) . . ?
C2 C1 P1 119.9(3) . . ?
C6 C1 P1 119.9(2) . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C8 C7 C12 119.4(3) . . ?
C8 C7 P1 118.6(2) . . ?
C12 C7 P1 121.9(2) . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120.7(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C7 120.3(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 N3 109.7(3) . . ?
N1 C13 P1 127.4(2) . . ?
N3 C13 P1 122.3(2) . . ?
N2 C14 N1 115.6(3) . . ?
N2 C14 H14 122.2 . . ?
N1 C14 H14 122.2 . . ?
N3 C15 N4 111.5(3) . . ?
N3 C15 H15A 109.3 . . ?
N4 C15 H15A 109.3 . . ?
N3 C15 H15B 109.3 . . ?
N4 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
N5 C16 N6 115.6(3) . . ?
N5 C16 H16 122.2 . . ?
N6 C16 H16 122.2 . . ?
N6 C17 N4 109.4(3) . . ?
N6 C17 P2 125.0(2) . . ?
N4 C17 P2 125.6(2) . . ?
C23 C18 C19 119.1(3) . . ?
C23 C18 P2 121.6(2) . . ?
C19 C18 P2 119.3(2) . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 119.6(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 120.6(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C18 120.1(3) . . ?
C22 C23 H23 119.9 . . ?
C18 C23 H23 119.9 . . ?
C29 C24 C25 120.3(3) . . ?
C29 C24 P2 124.2(2) . . ?
C25 C24 P2 115.3(2) . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.1(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 120.5(3) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C24 119.2(3) . . ?
C28 C29 H29 120.4 . . ?
C24 C29 H29 120.4 . . ?

_refine_diff_density_max         0.591
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.090

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_MSB578_0m
_database_code_depnum_ccdc_archive 'CCDC 1511158'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[1-({2-[diphenyl[selenylidene)-λ⁵-phosphanyl]-1H-imidazol-1-yl}methyl)-1H-imidazol-2-yl]diphenyl-λ⁵-phosphaselenone'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 N4 P2 Se2'
_chemical_formula_sum            'C31 H26 N4 P2 Se2'
_chemical_formula_weight         674.42

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.078(3)
_cell_length_b                   13.427(3)
_cell_length_c                   16.699(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.209(4)
_cell_angle_gamma                90
_cell_volume                     2854.9(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9516
_cell_measurement_theta_min      2.2043
_cell_measurement_theta_max      29.0476
_cell_measurement_temperature    100(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   0.330
_exptl_transmission_factor_max   0.473
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.147
_exptl_absorpt_coefficient_mu    2.731
_shelx_estimated_absorpt_T_min   0.558
_shelx_estimated_absorpt_T_max   0.690
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.69

_exptl_special_details           
;

The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            51765
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.792
_diffrn_reflns_theta_max         29.090
_diffrn_reflns_theta_full        28.500
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7522
_reflns_number_gt                6590
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2016)'

_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. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 - 0.99 Å). 
All were included as riding contributions with isotropic displacement 
parameters 1.2 - 1.5 times those of the attached atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+1.4840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7522
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.41842(2) 0.03291(2) 0.60950(2) 0.02146(6) Uani 1 1 d . . . . .
Se2 Se 0.09578(2) 0.41915(2) 0.31558(2) 0.01777(5) Uani 1 1 d . . . . .
P1 P 0.25382(3) 0.02829(3) 0.56750(3) 0.01156(9) Uani 1 1 d . . . . .
P2 P 0.23881(3) 0.46125(3) 0.39456(3) 0.01127(9) Uani 1 1 d . . . . .
N1 N 0.16182(11) -0.01718(11) 0.40458(8) 0.0149(3) Uani 1 1 d . . . . .
N2 N 0.22455(11) 0.13778(10) 0.41917(9) 0.0141(3) Uani 1 1 d . . . . .
N3 N 0.34162(11) 0.27635(10) 0.41893(9) 0.0139(3) Uani 1 1 d . . . . .
N4 N 0.42970(11) 0.39172(11) 0.36629(9) 0.0149(3) Uani 1 1 d . . . . .
C1 C 0.19626(13) -0.09186(12) 0.58016(10) 0.0129(3) Uani 1 1 d . . . . .
C2 C 0.23664(14) -0.17576(13) 0.54834(10) 0.0178(3) Uani 1 1 d . . . . .
H2 H 0.2932 -0.1689 0.5218 0.021 Uiso 1 1 calc R U . . .
C3 C 0.19397(15) -0.26904(13) 0.55567(11) 0.0207(4) Uani 1 1 d . . . . .
H3 H 0.2205 -0.3259 0.5333 0.025 Uiso 1 1 calc R U . . .
C4 C 0.11196(14) -0.27918(13) 0.59595(12) 0.0215(4) Uani 1 1 d . . . . .
H4 H 0.0827 -0.3430 0.6008 0.026 Uiso 1 1 calc R U . . .
C5 C 0.07320(13) -0.19674(13) 0.62881(11) 0.0195(4) Uani 1 1 d . . . . .
H5 H 0.0181 -0.2043 0.6569 0.023 Uiso 1 1 calc R U . . .
C6 C 0.11475(13) -0.10235(13) 0.62086(10) 0.0159(3) Uani 1 1 d . . . . .
H6 H 0.0877 -0.0456 0.6430 0.019 Uiso 1 1 calc R U . . .
C7 C 0.18440(12) 0.11941(12) 0.61513(10) 0.0122(3) Uani 1 1 d . . . . .
C8 C 0.23588(13) 0.16951(13) 0.68625(10) 0.0151(3) Uani 1 1 d . . . . .
H8 H 0.3088 0.1591 0.7082 0.018 Uiso 1 1 calc R U . . .
C9 C 0.17972(14) 0.23483(13) 0.72482(11) 0.0182(3) Uani 1 1 d . . . . .
H9 H 0.2143 0.2692 0.7732 0.022 Uiso 1 1 calc R U . . .
C10 C 0.07317(14) 0.24964(14) 0.69249(11) 0.0182(3) Uani 1 1 d . . . . .
H10 H 0.0350 0.2938 0.7193 0.022 Uiso 1 1 calc R U . . .
C11 C 0.02167(13) 0.20072(13) 0.62140(11) 0.0185(3) Uani 1 1 d . . . . .
H11 H -0.0512 0.2115 0.5996 0.022 Uiso 1 1 calc R U . . .
C12 C 0.07735(13) 0.13597(13) 0.58242(10) 0.0160(3) Uani 1 1 d . . . . .
H12 H 0.0427 0.1028 0.5335 0.019 Uiso 1 1 calc R U . . .
C13 C 0.20941(12) 0.05045(12) 0.45800(10) 0.0126(3) Uani 1 1 d . . . . .
C14 C 0.14555(14) 0.02843(13) 0.32875(10) 0.0169(3) Uani 1 1 d . . . . .
H14 H 0.1131 -0.0023 0.2781 0.020 Uiso 1 1 calc R U . . .
C15 C 0.18247(14) 0.12374(13) 0.33658(10) 0.0172(3) Uani 1 1 d . . . . .
H15 H 0.1797 0.1709 0.2937 0.021 Uiso 1 1 calc R U . . .
C16 C 0.26500(14) 0.23086(12) 0.45881(11) 0.0179(3) Uani 1 1 d . . . . .
H16A H 0.2983 0.2179 0.5173 0.021 Uiso 1 1 calc R U . . .
H16B H 0.2060 0.2777 0.4568 0.021 Uiso 1 1 calc R U . . .
C17 C 0.43202(13) 0.23156(13) 0.40800(11) 0.0178(3) Uani 1 1 d . . . . .
H17 H 0.4535 0.1647 0.4206 0.021 Uiso 1 1 calc R U . . .
C18 C 0.48452(13) 0.30304(14) 0.37538(11) 0.0180(3) Uani 1 1 d . . . . .
H18 H 0.5499 0.2931 0.3609 0.022 Uiso 1 1 calc R U . . .
C19 C 0.34384(12) 0.37341(12) 0.39315(10) 0.0125(3) Uani 1 1 d . . . . .
C20 C 0.28346(13) 0.58446(12) 0.37346(10) 0.0142(3) Uani 1 1 d . . . . .
C21 C 0.38704(15) 0.61652(14) 0.40110(12) 0.0230(4) Uani 1 1 d . . . . .
H21 H 0.4399 0.5707 0.4264 0.028 Uiso 1 1 calc R U . . .
C22 C 0.41286(16) 0.71588(15) 0.39153(12) 0.0265(4) Uani 1 1 d . . . . .
H22 H 0.4836 0.7375 0.4096 0.032 Uiso 1 1 calc R U . . .
C23 C 0.33563(17) 0.78318(14) 0.35569(11) 0.0245(4) Uani 1 1 d . . . . .
H23 H 0.3531 0.8512 0.3506 0.029 Uiso 1 1 calc R U . . .
C24 C 0.23303(16) 0.75135(14) 0.32729(12) 0.0242(4) Uani 1 1 d . . . . .
H24 H 0.1804 0.7975 0.3021 0.029 Uiso 1 1 calc R U . . .
C25 C 0.20678(14) 0.65208(13) 0.33557(11) 0.0192(3) Uani 1 1 d . . . . .
H25 H 0.1365 0.6304 0.3154 0.023 Uiso 1 1 calc R U . . .
C26 C 0.23543(13) 0.46485(12) 0.50300(10) 0.0124(3) Uani 1 1 d . . . . .
C27 C 0.32813(14) 0.48041(14) 0.56259(12) 0.0201(4) Uani 1 1 d . . . . .
H27 H 0.3928 0.4884 0.5465 0.024 Uiso 1 1 calc R U . . .
C28 C 0.32605(16) 0.48420(15) 0.64532(12) 0.0250(4) Uani 1 1 d . . . . .
H28 H 0.3891 0.4947 0.6858 0.030 Uiso 1 1 calc R U . . .
C29 C 0.23158(16) 0.47262(14) 0.66868(11) 0.0228(4) Uani 1 1 d . . . . .
H29 H 0.2301 0.4749 0.7253 0.027 Uiso 1 1 calc R U . . .
C30 C 0.13902(15) 0.45774(13) 0.60956(11) 0.0201(4) Uani 1 1 d . . . . .
H30 H 0.0744 0.4503 0.6258 0.024 Uiso 1 1 calc R U . . .
C31 C 0.14077(13) 0.45375(13) 0.52660(11) 0.0160(3) Uani 1 1 d . . . . .
H31 H 0.0775 0.4435 0.4862 0.019 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 P1 2.1072(7) . ?
Se2 P2 2.1049(6) . ?
P1 C7 1.8121(17) . ?
P1 C13 1.8123(17) . ?
P1 C1 1.8130(17) . ?
P2 C19 1.8147(17) . ?
P2 C20 1.8155(17) . ?
P2 C26 1.8222(18) . ?
N1 C13 1.325(2) . ?
N1 C14 1.379(2) . ?
N2 C13 1.376(2) . ?
N2 C15 1.376(2) . ?
N2 C16 1.456(2) . ?
N3 C19 1.375(2) . ?
N3 C17 1.375(2) . ?
N3 C16 1.458(2) . ?
N4 C19 1.324(2) . ?
N4 C18 1.380(2) . ?
C1 C6 1.396(2) . ?
C1 C2 1.399(2) . ?
C2 C3 1.388(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.397(2) . ?
C7 C12 1.399(2) . ?
C8 C9 1.393(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.363(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.364(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C20 C25 1.393(2) . ?
C20 C21 1.396(2) . ?
C21 C22 1.394(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.390(2) . ?
C26 C27 1.397(2) . ?
C27 C28 1.389(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.392(2) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
C7 P1 C13 104.76(7) . . ?
C7 P1 C1 106.66(8) . . ?
C13 P1 C1 102.59(7) . . ?
C7 P1 Se1 114.22(6) . . ?
C13 P1 Se1 113.48(5) . . ?
C1 P1 Se1 114.03(6) . . ?
C19 P2 C20 108.17(8) . . ?
C19 P2 C26 102.74(7) . . ?
C20 P2 C26 104.51(8) . . ?
C19 P2 Se2 112.60(6) . . ?
C20 P2 Se2 113.72(6) . . ?
C26 P2 Se2 114.19(6) . . ?
C13 N1 C14 105.32(14) . . ?
C13 N2 C15 106.74(14) . . ?
C13 N2 C16 126.42(14) . . ?
C15 N2 C16 126.43(14) . . ?
C19 N3 C17 107.02(14) . . ?
C19 N3 C16 127.30(14) . . ?
C17 N3 C16 125.37(15) . . ?
C19 N4 C18 105.19(14) . . ?
C6 C1 C2 120.00(15) . . ?
C6 C1 P1 122.01(13) . . ?
C2 C1 P1 117.99(13) . . ?
C3 C2 C1 119.92(17) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.93(17) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.31(16) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.19(17) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.64(16) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C8 C7 C12 120.02(15) . . ?
C8 C7 P1 120.39(12) . . ?
C12 C7 P1 119.53(12) . . ?
C9 C8 C7 119.59(15) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 119.91(16) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.80(16) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 119.55(16) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 120.12(16) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 N2 111.28(14) . . ?
N1 C13 P1 124.05(13) . . ?
N2 C13 P1 124.62(12) . . ?
C15 C14 N1 110.61(15) . . ?
C15 C14 H14 124.7 . . ?
N1 C14 H14 124.7 . . ?
C14 C15 N2 106.05(15) . . ?
C14 C15 H15 127.0 . . ?
N2 C15 H15 127.0 . . ?
N2 C16 N3 111.60(13) . . ?
N2 C16 H16A 109.3 . . ?
N3 C16 H16A 109.3 . . ?
N2 C16 H16B 109.3 . . ?
N3 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 N3 105.77(15) . . ?
C18 C17 H17 127.1 . . ?
N3 C17 H17 127.1 . . ?
C17 C18 N4 110.78(15) . . ?
C17 C18 H18 124.6 . . ?
N4 C18 H18 124.6 . . ?
N4 C19 N3 111.24(14) . . ?
N4 C19 P2 125.93(13) . . ?
N3 C19 P2 122.81(12) . . ?
C25 C20 C21 119.52(16) . . ?
C25 C20 P2 116.88(13) . . ?
C21 C20 P2 123.22(13) . . ?
C22 C21 C20 119.96(18) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 120.13(18) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.03(18) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.23(18) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 120.09(17) . . ?
C24 C25 H25 120.0 . . ?
C20 C25 H25 120.0 . . ?
C31 C26 C27 119.87(16) . . ?
C31 C26 P2 120.28(13) . . ?
C27 C26 P2 119.84(13) . . ?
C28 C27 C26 120.19(17) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C29 C28 C27 119.80(17) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.22(17) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C31 120.17(17) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C26 C31 C30 119.75(16) . . ?
C26 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C6 -0.53(16) . . . . ?
C13 P1 C1 C6 -110.37(14) . . . . ?
Se1 P1 C1 C6 126.50(13) . . . . ?
C7 P1 C1 C2 -179.93(13) . . . . ?
C13 P1 C1 C2 70.23(14) . . . . ?
Se1 P1 C1 C2 -52.90(14) . . . . ?
C6 C1 C2 C3 1.5(3) . . . . ?
P1 C1 C2 C3 -179.13(13) . . . . ?
C1 C2 C3 C4 -1.0(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C3 C4 C5 C6 1.0(3) . . . . ?
C2 C1 C6 C5 -0.7(2) . . . . ?
P1 C1 C6 C5 179.94(13) . . . . ?
C4 C5 C6 C1 -0.5(3) . . . . ?
C13 P1 C7 C8 -139.15(14) . . . . ?
C1 P1 C7 C8 112.54(14) . . . . ?
Se1 P1 C7 C8 -14.38(15) . . . . ?
C13 P1 C7 C12 43.84(15) . . . . ?
C1 P1 C7 C12 -64.46(15) . . . . ?
Se1 P1 C7 C12 168.62(11) . . . . ?
C12 C7 C8 C9 0.8(2) . . . . ?
P1 C7 C8 C9 -176.14(13) . . . . ?
C7 C8 C9 C10 0.1(3) . . . . ?
C8 C9 C10 C11 -0.6(3) . . . . ?
C9 C10 C11 C12 0.3(3) . . . . ?
C10 C11 C12 C7 0.7(3) . . . . ?
C8 C7 C12 C11 -1.2(2) . . . . ?
P1 C7 C12 C11 175.80(13) . . . . ?
C14 N1 C13 N2 -0.17(19) . . . . ?
C14 N1 C13 P1 -177.63(12) . . . . ?
C15 N2 C13 N1 0.79(19) . . . . ?
C16 N2 C13 N1 173.70(15) . . . . ?
C15 N2 C13 P1 178.23(12) . . . . ?
C16 N2 C13 P1 -8.9(2) . . . . ?
C7 P1 C13 N1 -120.81(15) . . . . ?
C1 P1 C13 N1 -9.55(16) . . . . ?
Se1 P1 C13 N1 113.94(13) . . . . ?
C7 P1 C13 N2 62.06(15) . . . . ?
C1 P1 C13 N2 173.33(14) . . . . ?
Se1 P1 C13 N2 -63.18(15) . . . . ?
C13 N1 C14 C15 -0.5(2) . . . . ?
N1 C14 C15 N2 1.0(2) . . . . ?
C13 N2 C15 C14 -1.07(18) . . . . ?
C16 N2 C15 C14 -173.98(15) . . . . ?
C13 N2 C16 N3 136.37(16) . . . . ?
C15 N2 C16 N3 -52.1(2) . . . . ?
C19 N3 C16 N2 130.43(17) . . . . ?
C17 N3 C16 N2 -56.8(2) . . . . ?
C19 N3 C17 C18 -0.57(19) . . . . ?
C16 N3 C17 C18 -174.53(16) . . . . ?
N3 C17 C18 N4 0.5(2) . . . . ?
C19 N4 C18 C17 -0.3(2) . . . . ?
C18 N4 C19 N3 -0.10(19) . . . . ?
C18 N4 C19 P2 -178.57(12) . . . . ?
C17 N3 C19 N4 0.43(19) . . . . ?
C16 N3 C19 N4 174.24(15) . . . . ?
C17 N3 C19 P2 178.96(12) . . . . ?
C16 N3 C19 P2 -7.2(2) . . . . ?
C20 P2 C19 N4 -11.76(17) . . . . ?
C26 P2 C19 N4 -121.91(15) . . . . ?
Se2 P2 C19 N4 114.78(14) . . . . ?
C20 P2 C19 N3 169.94(13) . . . . ?
C26 P2 C19 N3 59.78(15) . . . . ?
Se2 P2 C19 N3 -63.53(15) . . . . ?
C19 P2 C20 C25 151.56(13) . . . . ?
C26 P2 C20 C25 -99.49(14) . . . . ?
Se2 P2 C20 C25 25.69(15) . . . . ?
C19 P2 C20 C21 -35.58(18) . . . . ?
C26 P2 C20 C21 73.36(17) . . . . ?
Se2 P2 C20 C21 -161.46(14) . . . . ?
C25 C20 C21 C22 0.7(3) . . . . ?
P2 C20 C21 C22 -171.93(15) . . . . ?
C20 C21 C22 C23 0.9(3) . . . . ?
C21 C22 C23 C24 -1.7(3) . . . . ?
C22 C23 C24 C25 0.8(3) . . . . ?
C23 C24 C25 C20 0.8(3) . . . . ?
C21 C20 C25 C24 -1.6(3) . . . . ?
P2 C20 C25 C24 171.53(14) . . . . ?
C19 P2 C26 C31 -130.63(14) . . . . ?
C20 P2 C26 C31 116.49(14) . . . . ?
Se2 P2 C26 C31 -8.39(15) . . . . ?
C19 P2 C26 C27 50.39(15) . . . . ?
C20 P2 C26 C27 -62.49(15) . . . . ?
Se2 P2 C26 C27 172.63(12) . . . . ?
C31 C26 C27 C28 0.4(3) . . . . ?
P2 C26 C27 C28 179.38(14) . . . . ?
C26 C27 C28 C29 -0.1(3) . . . . ?
C27 C28 C29 C30 -0.3(3) . . . . ?
C28 C29 C30 C31 0.4(3) . . . . ?
C27 C26 C31 C30 -0.3(3) . . . . ?
P2 C26 C31 C30 -179.29(13) . . . . ?
C29 C30 C31 C26 -0.1(3) . . . . ?

_refine_diff_density_max         0.752
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_compound6_msb671_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1511159'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
1-({5-[diphenyl(selenylidene)-λ⁵-phosphanyl]-1H-1,2,4-triazol-1-yl}methyl)-1H-1,2,4-triazol-5-yldiphenyl-λ⁵-phosphaneselone
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H24 N6 P2 Se2'
_chemical_formula_sum            'C29 H24 N6 P2 Se2'
_chemical_formula_weight         676.40

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.321(3)
_cell_length_b                   11.432(2)
_cell_length_c                   17.924(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.979(2)
_cell_angle_gamma                90
_cell_volume                     2847.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9159
_cell_measurement_theta_min      2.3069
_cell_measurement_theta_max      27.0126

_exptl_crystal_description       column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   0.520
_exptl_transmission_factor_max   0.928
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.740
_shelx_estimated_absorpt_T_min   0.559
_shelx_estimated_absorpt_T_max   0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'

_exptl_special_details           
;
The diffraction data were collected in three sets of 606 frames 
(0.3° width in ω) at φ = 0, 120 and 240°. A scan time of 30 
sec/frame was used. Analysis of 1375 reflections having I/σ(I) > 14 
and chosen from the full data set with CELL_NOW (Sheldrick, 2008) 
showed the crystal to belong to the monoclinic system and to 
consist primarily of two components rotated from one another by 7.6° 
about the real axis  1.000 -0.216  0.216. The raw data were processed 
using the multi-component version of SAINT under control of the 
two-component orientation file generated by CELL_NOW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            9159
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.640
_diffrn_reflns_theta_max         27.123
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             42623
_reflns_number_gt                22031
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker AXS, 2013)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013a)'
_computing_structure_solution    'SHELXT (Bruker AXS 2013b)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

_refine_special_details          
;
H-atoms attached to carbon were placed in calculated positions 
(C---H = 0.95 - 0.98 Å). All were included as riding contributions 
with isotropic displacement parameters 1.2 - 1.5 times those of the 
attached atoms. The structure was refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1131P)²+2.5490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         42623
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0916
_refine_ls_wR_factor_ref         0.2846
_refine_ls_wR_factor_gt          0.2389
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.61284(7) -0.00229(8) 0.40735(6) 0.0376(3) Uani 1 1 d . . . . .
Se2 Se 0.17368(8) 0.11927(10) 0.34745(7) 0.0487(4) Uani 1 1 d . . . . .
P1 P 0.64277(15) 0.1779(2) 0.41030(12) 0.0243(5) Uani 1 1 d . . . . .
P2 P 0.17399(16) 0.2428(2) 0.43357(14) 0.0307(6) Uani 1 1 d . . . . .
N1 N 0.5379(5) 0.3478(7) 0.3128(4) 0.0316(18) Uani 1 1 d . . . . .
N2 N 0.3890(5) 0.3336(7) 0.3334(5) 0.038(2) Uani 1 1 d . . . . .
N3 N 0.4491(5) 0.2549(6) 0.3772(4) 0.0307(17) Uani 1 1 d . . . . .
N4 N 0.3810(5) 0.2506(7) 0.4851(5) 0.0379(19) Uani 1 1 d . . . . .
N5 N 0.4486(6) 0.3022(9) 0.5425(5) 0.049(2) Uani 1 1 d . . . . .
N6 N 0.3081(4) 0.3505(5) 0.5550(3) 0.0150(13) Uani 1 1 d . . . . .
C1 C 0.7301(6) 0.2203(8) 0.3575(5) 0.030(2) Uani 1 1 d . . . . .
C2 C 0.7517(7) 0.1416(11) 0.3047(6) 0.047(3) Uani 1 1 d . . . . .
H2 H 0.7239 0.0658 0.2990 0.057 Uiso 1 1 calc R U . . .
C3 C 0.8140(9) 0.1751(13) 0.2607(7) 0.063(4) Uani 1 1 d . . . . .
H3 H 0.8271 0.1224 0.2236 0.076 Uiso 1 1 calc R U . . .
C4 C 0.8565(8) 0.2808(12) 0.2695(6) 0.055(3) Uani 1 1 d . . . . .
H4 H 0.8992 0.3018 0.2386 0.066 Uiso 1 1 calc R U . . .
C5 C 0.8386(7) 0.3574(11) 0.3220(6) 0.050(3) Uani 1 1 d . . . . .
H5 H 0.8702 0.4311 0.3286 0.061 Uiso 1 1 calc R U . . .
C6 C 0.7740(7) 0.3289(9) 0.3666(6) 0.040(2) Uani 1 1 d . . . . .
H6 H 0.7606 0.3834 0.4026 0.049 Uiso 1 1 calc R U . . .
C7 C 0.6753(6) 0.2393(9) 0.5061(5) 0.032(2) Uani 1 1 d . . . . .
C8 C 0.7088(7) 0.1646(11) 0.5678(5) 0.045(3) Uani 1 1 d . . . . .
H8 H 0.7168 0.0835 0.5596 0.055 Uiso 1 1 calc R U . . .
C9 C 0.7304(8) 0.2100(16) 0.6415(6) 0.073(4) Uani 1 1 d . . . . .
H9 H 0.7526 0.1594 0.6841 0.087 Uiso 1 1 calc R U . . .
C10 C 0.7203(9) 0.3249(17) 0.6537(7) 0.074(5) Uani 1 1 d . . . . .
H10 H 0.7355 0.3543 0.7048 0.089 Uiso 1 1 calc R U . . .
C11 C 0.6881(8) 0.4008(13) 0.5931(8) 0.066(4) Uani 1 1 d . . . . .
H11 H 0.6827 0.4821 0.6023 0.079 Uiso 1 1 calc R U . . .
C12 C 0.6635(7) 0.3569(10) 0.5174(6) 0.043(3) Uani 1 1 d . . . . .
H12 H 0.6392 0.4075 0.4751 0.052 Uiso 1 1 calc R U . . .
C13 C 0.5385(6) 0.2646(7) 0.3649(5) 0.0254(18) Uani 1 1 d . . . . .
C14 C 0.4452(7) 0.3867(9) 0.2966(5) 0.038(2) Uani 1 1 d . . . . .
H14 H 0.4230 0.4482 0.2611 0.045 Uiso 1 1 calc R U . . .
C15 C 0.4136(7) 0.1806(8) 0.4302(6) 0.038(2) Uani 1 1 d . . . . .
H15A H 0.3599 0.1318 0.4011 0.045 Uiso 1 1 calc R U . . .
H15B H 0.4656 0.1278 0.4572 0.045 Uiso 1 1 calc R U . . .
C16 C 0.3972(8) 0.3643(11) 0.5794(6) 0.050(3) Uani 1 1 d . . . . .
H16 H 0.4248 0.4151 0.6208 0.060 Uiso 1 1 calc R U . . .
C17 C 0.2909(6) 0.2829(8) 0.4926(5) 0.034(2) Uani 1 1 d . . . . .
C18 C 0.1074(6) 0.1965(8) 0.5021(5) 0.0267(19) Uani 1 1 d . . . . .
C19 C 0.1451(6) 0.1770(8) 0.5791(5) 0.034(2) Uani 1 1 d . . . . .
H19 H 0.2113 0.1914 0.6013 0.041 Uiso 1 1 calc R U . . .
C20 C 0.0861(7) 0.1362(9) 0.6243(6) 0.039(2) Uani 1 1 d . . . . .
H20 H 0.1118 0.1232 0.6776 0.047 Uiso 1 1 calc R U . . .
C21 C -0.0099(8) 0.1145(8) 0.5919(6) 0.043(3) Uani 1 1 d . . . . .
H21 H -0.0500 0.0868 0.6233 0.052 Uiso 1 1 calc R U . . .
C22 C -0.0470(7) 0.1321(8) 0.5171(6) 0.037(2) Uani 1 1 d . . . . .
H22 H -0.1131 0.1162 0.4956 0.044 Uiso 1 1 calc R U . . .
C23 C 0.0099(6) 0.1733(8) 0.4704(6) 0.032(2) Uani 1 1 d . . . . .
H23 H -0.0171 0.1857 0.4172 0.038 Uiso 1 1 calc R U . . .
C24 C 0.1235(6) 0.3812(8) 0.3959(5) 0.029(2) Uani 1 1 d . . . . .
C25 C 0.1090(7) 0.4034(9) 0.3179(6) 0.041(2) Uani 1 1 d . . . . .
H25 H 0.1271 0.3470 0.2851 0.050 Uiso 1 1 calc R U . . .
C26 C 0.0672(8) 0.5096(12) 0.2878(7) 0.060(4) Uani 1 1 d . . . . .
H26 H 0.0567 0.5248 0.2343 0.072 Uiso 1 1 calc R U . . .
C27 C 0.0419(8) 0.5906(11) 0.3341(8) 0.054(3) Uani 1 1 d . . . . .
H27 H 0.0148 0.6629 0.3133 0.065 Uiso 1 1 calc R U . . .
C28 C 0.0553(7) 0.5684(10) 0.4108(7) 0.050(3) Uani 1 1 d . . . . .
H28 H 0.0356 0.6247 0.4428 0.060 Uiso 1 1 calc R U . . .
C29 C 0.0973(6) 0.4648(9) 0.4426(6) 0.035(2) Uani 1 1 d . . . . .
H29 H 0.1080 0.4514 0.4963 0.042 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 P1 2.102(3) . ?
Se2 P2 2.091(3) . ?
P1 C1 1.806(9) . ?
P1 C7 1.809(9) . ?
P1 C13 1.813(8) . ?
P2 C24 1.802(9) . ?
P2 C18 1.806(8) . ?
P2 C17 1.811(9) . ?
N1 C13 1.331(11) . ?
N1 C14 1.364(11) . ?
N2 C14 1.306(12) . ?
N2 N3 1.357(10) . ?
N3 C13 1.355(10) . ?
N3 C15 1.454(11) . ?
N4 N5 1.364(11) . ?
N4 C17 1.379(11) . ?
N4 C15 1.433(12) . ?
N5 C16 1.311(14) . ?
N6 C16 1.255(12) . ?
N6 C17 1.332(11) . ?
C1 C6 1.384(13) . ?
C1 C2 1.395(13) . ?
C2 C3 1.378(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.345(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.355(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(13) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.377(14) . ?
C7 C8 1.388(14) . ?
C8 C9 1.384(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.35(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.38(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.409(15) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16 0.9500 . ?
C18 C19 1.374(12) . ?
C18 C23 1.400(11) . ?
C19 C20 1.385(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.379(14) . ?
C20 H20 0.9500 . ?
C21 C22 1.333(14) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(13) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.381(13) . ?
C24 C25 1.386(13) . ?
C25 C26 1.403(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.349(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.365(16) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(14) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

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
C1 P1 C7 109.9(4) . . ?
C1 P1 C13 102.6(4) . . ?
C7 P1 C13 102.1(4) . . ?
C1 P1 Se1 114.3(3) . . ?
C7 P1 Se1 114.1(3) . . ?
C13 P1 Se1 112.5(3) . . ?
C24 P2 C18 106.4(4) . . ?
C24 P2 C17 103.1(4) . . ?
C18 P2 C17 104.1(4) . . ?
C24 P2 Se2 112.8(3) . . ?
C18 P2 Se2 113.4(3) . . ?
C17 P2 Se2 116.1(3) . . ?
C13 N1 C14 102.9(7) . . ?
C14 N2 N3 102.6(7) . . ?
C13 N3 N2 110.1(7) . . ?
C13 N3 C15 130.3(7) . . ?
N2 N3 C15 119.5(7) . . ?
N5 N4 C17 108.7(8) . . ?
N5 N4 C15 118.1(8) . . ?
C17 N4 C15 133.2(8) . . ?
C16 N5 N4 103.4(8) . . ?
C16 N6 C17 109.4(8) . . ?
C6 C1 C2 119.3(9) . . ?
C6 C1 P1 122.1(7) . . ?
C2 C1 P1 118.6(7) . . ?
C3 C2 C1 119.4(11) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C4 C3 C2 121.3(12) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 120.4(10) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.6(11) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.1(10) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C12 C7 C8 121.0(9) . . ?
C12 C7 P1 120.4(8) . . ?
C8 C7 P1 118.6(8) . . ?
C9 C8 C7 119.0(13) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C10 C9 C8 120.9(13) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 120.9(11) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 119.5(13) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C7 C12 C11 118.6(11) . . ?
C7 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N1 C13 N3 109.1(7) . . ?
N1 C13 P1 124.8(6) . . ?
N3 C13 P1 126.2(7) . . ?
N2 C14 N1 115.4(8) . . ?
N2 C14 H14 122.3 . . ?
N1 C14 H14 122.3 . . ?
N4 C15 N3 110.2(8) . . ?
N4 C15 H15A 109.6 . . ?
N3 C15 H15A 109.6 . . ?
N4 C15 H15B 109.6 . . ?
N3 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N6 C16 N5 113.8(10) . . ?
N6 C16 H16 123.1 . . ?
N5 C16 H16 123.1 . . ?
N6 C17 N4 104.5(8) . . ?
N6 C17 P2 126.5(6) . . ?
N4 C17 P2 129.1(8) . . ?
C19 C18 C23 119.2(8) . . ?
C19 C18 P2 126.0(7) . . ?
C23 C18 P2 114.8(7) . . ?
C18 C19 C20 119.7(9) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 120.1(9) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.7(9) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.6(9) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C18 119.7(9) . . ?
C22 C23 H23 120.1 . . ?
C18 C23 H23 120.1 . . ?
C29 C24 C25 119.2(9) . . ?
C29 C24 P2 121.6(7) . . ?
C25 C24 P2 119.2(8) . . ?
C24 C25 C26 119.5(11) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 120.6(11) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 119.9(11) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C29 121.0(11) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C24 C29 C28 119.7(10) . . ?
C24 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?

_refine_diff_density_max         2.088
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.271

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_compound10_MSB619_0m
_database_code_depnum_ccdc_archive 'CCDC 1511160'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
Chlorido(η⁵-cyclopentadienyl)(2-(diphenylphosphanyl)-1-{[2-(diphenylphosphanyl)-1H-imidazol-1-yl]methyl}-1H-imidazole-κ²P,P')ruthenium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H31 Cl N4 P2 Ru'
_chemical_formula_sum            'C36 H31 Cl N4 P2 Ru'
_chemical_formula_weight         718.11

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'
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/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.0252(13)
_cell_length_b                   25.073(3)
_cell_length_c                   11.0932(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.325(2)
_cell_angle_gamma                90
_cell_volume                     3066.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9410
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      29.14

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   0.904
_exptl_transmission_factor_max   0.943
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.737
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 15 sec/frame.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54370
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.007
_diffrn_reflns_theta_max         29.141
_diffrn_reflns_theta_full        28.750
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             8058
_reflns_number_gt                6920
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'

_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. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+2.4237P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8058
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.06517(2) 0.11465(2) 0.28514(2) 0.01141(5) Uani 1 1 d . . . . .
Cl1 Cl 0.04194(4) 0.20837(2) 0.33974(4) 0.01585(9) Uani 1 1 d . . . . .
P1 P 0.11442(4) 0.13794(2) 0.09230(4) 0.01285(10) Uani 1 1 d . . . . .
P2 P 0.26056(4) 0.11004(2) 0.35716(4) 0.01189(10) Uani 1 1 d . . . . .
N1 N 0.13498(16) 0.22998(7) -0.04657(15) 0.0194(3) Uani 1 1 d . . . . .
N2 N 0.25571(15) 0.23431(6) 0.11417(15) 0.0157(3) Uani 1 1 d . . . . .
N3 N 0.40067(15) 0.17690(6) 0.21048(14) 0.0154(3) Uani 1 1 d . . . . .
N4 N 0.47991(15) 0.09582(7) 0.22773(15) 0.0175(3) Uani 1 1 d . . . . .
C6 C -0.01862(18) 0.13853(7) -0.00781(17) 0.0162(4) Uani 1 1 d . . . . .
C1 C -0.05867(18) 0.05185(8) 0.22215(19) 0.0216(4) Uani 1 1 d . . . . .
H1 H -0.0646 0.0410 0.1403 0.026 Uiso 1 1 calc R U . . .
C2 C 0.02258(19) 0.03016(8) 0.31002(19) 0.0199(4) Uani 1 1 d . . . . .
H2 H 0.0813 0.0031 0.2969 0.024 Uiso 1 1 calc R U . . .
C3 C -0.00097(19) 0.05684(8) 0.42183(19) 0.0202(4) Uani 1 1 d . . . . .
H3 H 0.0383 0.0500 0.4967 0.024 Uiso 1 1 calc R U . . .
C4 C -0.09247(19) 0.09482(8) 0.40086(19) 0.0209(4) Uani 1 1 d . . . . .
H4 H -0.1248 0.1183 0.4596 0.025 Uiso 1 1 calc R U . . .
C5 C -0.12932(18) 0.09249(9) 0.2773(2) 0.0223(4) Uani 1 1 d . . . . .
H5 H -0.1894 0.1139 0.2393 0.027 Uiso 1 1 calc R U . . .
C7 C -0.11511(18) 0.17150(8) 0.02571(18) 0.0186(4) Uani 1 1 d . . . . .
H7 H -0.1111 0.1906 0.0996 0.022 Uiso 1 1 calc R U . . .
C8 C -0.21686(19) 0.17650(8) -0.0483(2) 0.0214(4) Uani 1 1 d . . . . .
H8 H -0.2810 0.1997 -0.0260 0.026 Uiso 1 1 calc R U . . .
C9 C -0.2244(2) 0.14761(8) -0.1543(2) 0.0243(4) Uani 1 1 d . . . . .
H9 H -0.2944 0.1506 -0.2042 0.029 Uiso 1 1 calc R U . . .
C10 C -0.1298(2) 0.11423(8) -0.1881(2) 0.0263(5) Uani 1 1 d . . . . .
H10 H -0.1355 0.0944 -0.2608 0.032 Uiso 1 1 calc R U . . .
C11 C -0.0265(2) 0.10986(8) -0.11522(19) 0.0214(4) Uani 1 1 d . . . . .
H11 H 0.0384 0.0873 -0.1389 0.026 Uiso 1 1 calc R U . . .
C12 C 0.22201(18) 0.09457(8) 0.01407(17) 0.0162(4) Uani 1 1 d . . . . .
C13 C 0.21449(19) 0.03942(8) 0.03403(19) 0.0210(4) Uani 1 1 d . . . . .
H13 H 0.1547 0.0258 0.0871 0.025 Uiso 1 1 calc R U . . .
C14 C 0.2937(2) 0.00457(9) -0.0231(2) 0.0253(5) Uani 1 1 d . . . . .
H14 H 0.2878 -0.0327 -0.0088 0.030 Uiso 1 1 calc R U . . .
C15 C 0.3813(2) 0.02405(9) -0.10096(19) 0.0265(5) Uani 1 1 d . . . . .
H15 H 0.4357 0.0003 -0.1398 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3887(2) 0.07863(10) -0.1217(2) 0.0302(5) Uani 1 1 d . . . . .
H16 H 0.4481 0.0922 -0.1753 0.036 Uiso 1 1 calc R U . . .
C17 C 0.3095(2) 0.11366(8) -0.0643(2) 0.0230(4) Uani 1 1 d . . . . .
H17 H 0.3155 0.1509 -0.0789 0.028 Uiso 1 1 calc R U . . .
C18 C 0.17021(18) 0.20480(7) 0.05285(17) 0.0155(4) Uani 1 1 d . . . . .
C19 C 0.19992(19) 0.27676(8) -0.04902(19) 0.0217(4) Uani 1 1 d . . . . .
H19 H 0.1935 0.3031 -0.1103 0.026 Uiso 1 1 calc R U . . .
C20 C 0.27460(19) 0.27995(8) 0.04865(19) 0.0211(4) Uani 1 1 d . . . . .
H20 H 0.3290 0.3081 0.0677 0.025 Uiso 1 1 calc R U . . .
C21 C 0.31899(18) 0.22180(7) 0.22600(17) 0.0158(4) Uani 1 1 d . . . . .
H21A H 0.3659 0.2534 0.2529 0.019 Uiso 1 1 calc R U . . .
H21B H 0.2590 0.2132 0.2892 0.019 Uiso 1 1 calc R U . . .
C22 C 0.50461(18) 0.17707(8) 0.14260(18) 0.0194(4) Uani 1 1 d . . . . .
H22 H 0.5371 0.2060 0.0978 0.023 Uiso 1 1 calc R U . . .
C23 C 0.55128(18) 0.12679(8) 0.15333(19) 0.0198(4) Uani 1 1 d . . . . .
H23 H 0.6230 0.1148 0.1149 0.024 Uiso 1 1 calc R U . . .
C24 C 0.38908(17) 0.12729(7) 0.26058(17) 0.0143(4) Uani 1 1 d . . . . .
C25 C 0.29076(17) 0.15130(7) 0.48997(16) 0.0142(3) Uani 1 1 d . . . . .
C26 C 0.19572(18) 0.16099(8) 0.57020(17) 0.0166(4) Uani 1 1 d . . . . .
H26 H 0.1163 0.1487 0.5514 0.020 Uiso 1 1 calc R U . . .
C27 C 0.21666(19) 0.18849(8) 0.67722(18) 0.0199(4) Uani 1 1 d . . . . .
H27 H 0.1522 0.1946 0.7319 0.024 Uiso 1 1 calc R U . . .
C28 C 0.33258(19) 0.20685(8) 0.70337(18) 0.0204(4) Uani 1 1 d . . . . .
H28 H 0.3471 0.2258 0.7761 0.024 Uiso 1 1 calc R U . . .
C29 C 0.42704(19) 0.19782(8) 0.62467(18) 0.0194(4) Uani 1 1 d . . . . .
H29 H 0.5062 0.2104 0.6437 0.023 Uiso 1 1 calc R U . . .
C30 C 0.40631(19) 0.17032(7) 0.51750(18) 0.0176(4) Uani 1 1 d . . . . .
H30 H 0.4711 0.1645 0.4630 0.021 Uiso 1 1 calc R U . . .
C31 C 0.30751(16) 0.04397(7) 0.41024(17) 0.0146(4) Uani 1 1 d . . . . .
C32 C 0.31547(18) 0.03303(8) 0.53312(18) 0.0178(4) Uani 1 1 d . . . . .
H32 H 0.2988 0.0603 0.5902 0.021 Uiso 1 1 calc R U . . .
C33 C 0.34792(19) -0.01782(8) 0.5725(2) 0.0224(4) Uani 1 1 d . . . . .
H33 H 0.3540 -0.0251 0.6564 0.027 Uiso 1 1 calc R U . . .
C34 C 0.37133(19) -0.05781(8) 0.4896(2) 0.0251(5) Uani 1 1 d . . . . .
H34 H 0.3937 -0.0924 0.5166 0.030 Uiso 1 1 calc R U . . .
C35 C 0.36221(18) -0.04733(8) 0.3685(2) 0.0220(4) Uani 1 1 d . . . . .
H35 H 0.3776 -0.0750 0.3121 0.026 Uiso 1 1 calc R U . . .
C36 C 0.33072(18) 0.00338(8) 0.32701(19) 0.0191(4) Uani 1 1 d . . . . .
H36 H 0.3251 0.0103 0.2430 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C2 2.1877(19) . ?
Ru1 C1 2.1956(19) . ?
Ru1 C5 2.216(2) . ?
Ru1 C4 2.223(2) . ?
Ru1 C3 2.2237(19) . ?
Ru1 P1 2.2859(5) . ?
Ru1 P2 2.2962(5) . ?
Ru1 Cl1 2.4405(5) . ?
P1 C12 1.831(2) . ?
P1 C6 1.835(2) . ?
P1 C18 1.8394(19) . ?
P2 C25 1.8292(19) . ?
P2 C31 1.8319(19) . ?
P2 C24 1.833(2) . ?
N1 C18 1.327(2) . ?
N1 C19 1.375(3) . ?
N2 C20 1.372(2) . ?
N2 C18 1.375(3) . ?
N2 C21 1.454(2) . ?
N3 C24 1.368(2) . ?
N3 C22 1.375(2) . ?
N3 C21 1.453(2) . ?
N4 C24 1.328(2) . ?
N4 C23 1.382(3) . ?
C6 C11 1.394(3) . ?
C6 C7 1.399(3) . ?
C1 C5 1.423(3) . ?
C1 C2 1.428(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.434(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.429(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C7 C8 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.384(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.387(3) . ?
C12 C13 1.403(3) . ?
C13 C14 1.391(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.395(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C19 C20 1.359(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.367(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C25 C30 1.393(3) . ?
C25 C26 1.400(3) . ?
C26 C27 1.391(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.393(3) . ?
C31 C36 1.399(3) . ?
C32 C33 1.394(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.372(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.396(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?

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
C2 Ru1 C1 38.02(8) . . ?
C2 Ru1 C5 63.50(8) . . ?
C1 Ru1 C5 37.62(8) . . ?
C2 Ru1 C4 62.70(8) . . ?
C1 Ru1 C4 62.39(8) . . ?
C5 Ru1 C4 37.54(8) . . ?
C2 Ru1 C3 37.93(8) . . ?
C1 Ru1 C3 62.86(8) . . ?
C5 Ru1 C3 62.77(8) . . ?
C4 Ru1 C3 36.86(8) . . ?
C2 Ru1 P1 114.69(6) . . ?
C1 Ru1 P1 92.06(6) . . ?
C5 Ru1 P1 105.20(6) . . ?
C4 Ru1 P1 142.02(6) . . ?
C3 Ru1 P1 152.28(6) . . ?
C2 Ru1 P2 96.26(6) . . ?
C1 Ru1 P2 130.93(6) . . ?
C5 Ru1 P2 155.03(6) . . ?
C4 Ru1 P2 121.52(6) . . ?
C3 Ru1 P2 92.32(6) . . ?
P1 Ru1 P2 96.379(18) . . ?
C2 Ru1 Cl1 151.42(6) . . ?
C1 Ru1 Cl1 134.71(6) . . ?
C5 Ru1 Cl1 98.53(6) . . ?
C4 Ru1 Cl1 89.35(5) . . ?
C3 Ru1 Cl1 115.03(6) . . ?
P1 Ru1 Cl1 90.694(17) . . ?
P2 Ru1 Cl1 93.536(16) . . ?
C12 P1 C6 103.63(9) . . ?
C12 P1 C18 102.13(9) . . ?
C6 P1 C18 96.65(9) . . ?
C12 P1 Ru1 116.73(6) . . ?
C6 P1 Ru1 112.03(7) . . ?
C18 P1 Ru1 122.48(6) . . ?
C25 P2 C31 101.70(9) . . ?
C25 P2 C24 101.51(9) . . ?
C31 P2 C24 100.56(9) . . ?
C25 P2 Ru1 114.70(6) . . ?
C31 P2 Ru1 114.85(6) . . ?
C24 P2 Ru1 120.77(6) . . ?
C18 N1 C19 105.80(17) . . ?
C20 N2 C18 106.99(16) . . ?
C20 N2 C21 123.93(17) . . ?
C18 N2 C21 129.07(16) . . ?
C24 N3 C22 107.78(16) . . ?
C24 N3 C21 126.65(16) . . ?
C22 N3 C21 125.57(16) . . ?
C24 N4 C23 105.24(16) . . ?
C11 C6 C7 119.20(18) . . ?
C11 C6 P1 124.00(15) . . ?
C7 C6 P1 116.77(15) . . ?
C5 C1 C2 108.79(19) . . ?
C5 C1 Ru1 71.98(12) . . ?
C2 C1 Ru1 70.69(11) . . ?
C5 C1 H1 125.6 . . ?
C2 C1 H1 125.6 . . ?
Ru1 C1 H1 123.3 . . ?
C1 C2 C3 107.27(18) . . ?
C1 C2 Ru1 71.29(11) . . ?
C3 C2 Ru1 72.39(11) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 H2 126.4 . . ?
Ru1 C2 H2 121.7 . . ?
C4 C3 C2 107.82(18) . . ?
C4 C3 Ru1 71.54(11) . . ?
C2 C3 Ru1 69.67(11) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
Ru1 C3 H3 124.3 . . ?
C3 C4 C5 109.33(19) . . ?
C3 C4 Ru1 71.60(11) . . ?
C5 C4 Ru1 70.98(11) . . ?
C3 C4 H4 125.3 . . ?
C5 C4 H4 125.3 . . ?
Ru1 C4 H4 123.7 . . ?
C1 C5 C4 106.76(18) . . ?
C1 C5 Ru1 70.39(11) . . ?
C4 C5 Ru1 71.47(11) . . ?
C1 C5 H5 126.6 . . ?
C4 C5 H5 126.6 . . ?
Ru1 C5 H5 123.2 . . ?
C8 C7 C6 120.54(19) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C7 119.88(19) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.22(19) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 120.1(2) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C6 C11 C10 120.1(2) . . ?
C6 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C17 C12 C13 118.75(18) . . ?
C17 C12 P1 123.12(15) . . ?
C13 C12 P1 118.13(15) . . ?
C14 C13 C12 120.6(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 120.2(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 119.4(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C17 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C12 C17 C16 120.5(2) . . ?
C12 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
N1 C18 N2 110.60(17) . . ?
N1 C18 P1 122.31(15) . . ?
N2 C18 P1 127.00(14) . . ?
C20 C19 N1 110.34(18) . . ?
C20 C19 H19 124.8 . . ?
N1 C19 H19 124.8 . . ?
C19 C20 N2 106.27(18) . . ?
C19 C20 H20 126.9 . . ?
N2 C20 H20 126.9 . . ?
N3 C21 N2 111.15(15) . . ?
N3 C21 H21A 109.4 . . ?
N2 C21 H21A 109.4 . . ?
N3 C21 H21B 109.4 . . ?
N2 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 N3 105.31(17) . . ?
C23 C22 H22 127.3 . . ?
N3 C22 H22 127.3 . . ?
C22 C23 N4 110.79(18) . . ?
C22 C23 H23 124.6 . . ?
N4 C23 H23 124.6 . . ?
N4 C24 N3 110.88(17) . . ?
N4 C24 P2 127.37(15) . . ?
N3 C24 P2 121.74(14) . . ?
C30 C25 C26 119.23(17) . . ?
C30 C25 P2 122.17(15) . . ?
C26 C25 P2 118.47(14) . . ?
C27 C26 C25 120.49(18) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 119.41(19) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 120.68(19) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 120.01(19) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.16(19) . . ?
C29 C30 H30 119.9 . . ?
C25 C30 H30 119.9 . . ?
C32 C31 C36 119.48(18) . . ?
C32 C31 P2 120.59(15) . . ?
C36 C31 P2 119.88(15) . . ?
C31 C32 C33 120.11(19) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 119.89(19) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.95(19) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 119.42(19) . . ?
C35 C36 H36 120.3 . . ?
C31 C36 H36 120.3 . . ?

_refine_diff_density_max         0.781
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_compound5_msb640_0m
_database_code_depnum_ccdc_archive 'CCDC 1511161'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'[1-({3-diphenyl(selenylidene)-λ⁵-phosphanyl]-1H-pyrazol-1-yl}methyl)-1H-pyrazol-3-yl]diphenyl-λ⁵-phosphaselenone'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 N4 P2 Se2'
_chemical_formula_sum            'C31 H26 N4 P2 Se2'
_chemical_formula_weight         674.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 '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                   17.6873(6)
_cell_length_b                   9.4183(3)
_cell_length_c                   18.1538(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.520(1)
_cell_angle_gamma                90
_cell_volume                     2850.29(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9969
_cell_measurement_theta_min      4.9594
_cell_measurement_theta_max      72.4473

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   0.663
_exptl_transmission_factor_max   0.902
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.527
_shelx_estimated_absorpt_T_min   0.465
_shelx_estimated_absorpt_T_max   0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.84

_exptl_special_details           
;
Analysis of 1029 reflections having I/σ(I) > 15 and chosen 
from the full data set with CELL_NOW (Sheldrick, 2008a) 
showed the crystal to belong to the monoclinic system and 
to be twinned by a 180 ° rotation about c.
The raw data were processed using the multi-component version of
SAINT under control of the two-component orientation file
generated by CELL_NOW.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            50790
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.650
_diffrn_reflns_theta_max         72.440
_diffrn_reflns_theta_full        72.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             48861
_reflns_number_gt                43796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker AXS, 2013)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction        'SAINT  (Bruker AXS, 2013a)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

_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. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms. The final model was refined as a 2-component 
twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0281P)²+1.2489P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         48861
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Se1 Se 0.40503(2) 0.91541(3) 0.37918(2) 0.01903(9) Uani 1 1 d . . . . .
Se2 Se 0.11907(2) 0.37977(3) 0.14074(2) 0.02049(9) Uani 1 1 d . . . . .
P1 P 0.43155(4) 0.73147(7) 0.32652(4) 0.01233(15) Uani 1 1 d . . . . .
P2 P 0.06848(4) 0.54134(7) 0.18969(4) 0.01366(15) Uani 1 1 d . . . . .
N1 N 0.29940(12) 0.7125(2) 0.18877(13) 0.0149(5) Uani 1 1 d . . . . .
N2 N 0.27586(13) 0.6999(3) 0.11010(13) 0.0182(5) Uani 1 1 d . . . . .
N3 N 0.16618(12) 0.7734(2) 0.18311(13) 0.0157(5) Uani 1 1 d . . . . .
N4 N 0.16621(13) 0.9081(2) 0.15718(14) 0.0188(5) Uani 1 1 d . . . . .
C1 C 0.53717(15) 0.7166(3) 0.33722(15) 0.0132(5) Uani 1 1 d . . . . .
C2 C 0.58934(16) 0.8262(3) 0.37343(16) 0.0162(6) Uani 1 1 d . . . . .
H2 H 0.5693 0.9097 0.3897 0.019 Uiso 1 1 calc R U . . .
C3 C 0.67069(16) 0.8125(3) 0.38557(17) 0.0203(6) Uani 1 1 d . . . . .
H3 H 0.7062 0.8879 0.4091 0.024 Uiso 1 1 calc R U . . .
C4 C 0.70041(16) 0.6895(3) 0.36362(17) 0.0193(6) Uani 1 1 d . . . . .
H4 H 0.7564 0.6800 0.3734 0.023 Uiso 1 1 calc R U . . .
C5 C 0.64890(16) 0.5803(3) 0.32750(17) 0.0178(6) Uani 1 1 d . . . . .
H5 H 0.6694 0.4964 0.3121 0.021 Uiso 1 1 calc R U . . .
C6 C 0.56704(16) 0.5939(3) 0.31379(16) 0.0156(6) Uani 1 1 d . . . . .
H6 H 0.5315 0.5196 0.2885 0.019 Uiso 1 1 calc R U . . .
C7 C 0.40440(14) 0.5674(3) 0.36344(16) 0.0131(5) Uani 1 1 d . . . . .
C8 C 0.40400(16) 0.5622(3) 0.44016(16) 0.0180(6) Uani 1 1 d . . . . .
H8 H 0.4150 0.6454 0.4715 0.022 Uiso 1 1 calc R U . . .
C9 C 0.38742(16) 0.4351(3) 0.47060(17) 0.0212(6) Uani 1 1 d . . . . .
H9 H 0.3869 0.4316 0.5227 0.025 Uiso 1 1 calc R U . . .
C10 C 0.37167(17) 0.3139(3) 0.42512(18) 0.0228(7) Uani 1 1 d . . . . .
H10 H 0.3616 0.2267 0.4465 0.027 Uiso 1 1 calc R U . . .
C11 C 0.37054(17) 0.3187(3) 0.34862(18) 0.0221(6) Uani 1 1 d . . . . .
H11 H 0.3588 0.2353 0.3174 0.026 Uiso 1 1 calc R U . . .
C12 C 0.38657(16) 0.4450(3) 0.31736(17) 0.0186(6) Uani 1 1 d . . . . .
H12 H 0.3854 0.4482 0.2647 0.022 Uiso 1 1 calc R U . . .
C13 C 0.38123(14) 0.7195(3) 0.22244(16) 0.0135(5) Uani 1 1 d . . . . .
C14 C 0.41149(16) 0.7129(3) 0.16161(16) 0.0163(6) Uani 1 1 d . . . . .
H14 H 0.4662 0.7154 0.1649 0.020 Uiso 1 1 calc R U . . .
C15 C 0.34383(16) 0.7017(3) 0.09388(17) 0.0179(6) Uani 1 1 d . . . . .
H15 H 0.3463 0.6962 0.0425 0.022 Uiso 1 1 calc R U . . .
C16 C 0.24080(15) 0.7072(3) 0.22937(16) 0.0189(6) Uani 1 1 d . . . . .
H16A H 0.2307 0.6071 0.2398 0.023 Uiso 1 1 calc R U . . .
H16B H 0.2626 0.7568 0.2802 0.023 Uiso 1 1 calc R U . . .
C17 C 0.08899(16) 0.9358(3) 0.11935(17) 0.0194(6) Uani 1 1 d . . . . .
H17 H 0.0699 1.0231 0.0936 0.023 Uiso 1 1 calc R U . . .
C18 C 0.03940(16) 0.8218(3) 0.12191(16) 0.0176(6) Uani 1 1 d . . . . .
H18 H -0.0174 0.8171 0.0996 0.021 Uiso 1 1 calc R U . . .
C19 C 0.09052(15) 0.7175(3) 0.16376(16) 0.0147(6) Uani 1 1 d . . . . .
C20 C 0.10343(15) 0.5382(3) 0.29581(16) 0.0150(6) Uani 1 1 d . . . . .
C21 C 0.08729(17) 0.6499(3) 0.33889(18) 0.0217(6) Uani 1 1 d . . . . .
H21 H 0.0570 0.7294 0.3127 0.026 Uiso 1 1 calc R U . . .
C22 C 0.11551(19) 0.6448(3) 0.41984(18) 0.0270(7) Uani 1 1 d . . . . .
H22 H 0.1038 0.7201 0.4492 0.032 Uiso 1 1 calc R U . . .
C23 C 0.16090(17) 0.5297(3) 0.45817(18) 0.0250(7) Uani 1 1 d . . . . .
H23 H 0.1811 0.5274 0.5137 0.030 Uiso 1 1 calc R U . . .
C24 C 0.17667(16) 0.4191(3) 0.41609(17) 0.0223(7) Uani 1 1 d . . . . .
H24 H 0.2070 0.3399 0.4426 0.027 Uiso 1 1 calc R U . . .
C25 C 0.14824(15) 0.4226(3) 0.33465(17) 0.0179(6) Uani 1 1 d . . . . .
H25 H 0.1594 0.3463 0.3057 0.021 Uiso 1 1 calc R U . . .
C26 C -0.04038(15) 0.5382(3) 0.15376(17) 0.0149(6) Uani 1 1 d . . . . .
C27 C -0.08647(16) 0.5502(3) 0.20247(17) 0.0186(6) Uani 1 1 d . . . . .
H27 H -0.0614 0.5663 0.2569 0.022 Uiso 1 1 calc R U . . .
C28 C -0.16954(16) 0.5386(3) 0.17076(18) 0.0226(7) Uani 1 1 d . . . . .
H28 H -0.2013 0.5465 0.2036 0.027 Uiso 1 1 calc R U . . .
C29 C -0.20594(16) 0.5155(3) 0.09156(18) 0.0218(7) Uani 1 1 d . . . . .
H29 H -0.2626 0.5059 0.0705 0.026 Uiso 1 1 calc R U . . .
C30 C -0.16050(16) 0.5063(3) 0.04283(18) 0.0219(6) Uani 1 1 d . . . . .
H30 H -0.1860 0.4923 -0.0117 0.026 Uiso 1 1 calc R U . . .
C31 C -0.07761(16) 0.5176(3) 0.07372(17) 0.0192(6) Uani 1 1 d . . . . .
H31 H -0.0463 0.5114 0.0403 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 P1 2.1059(8) . ?
Se2 P2 2.1064(8) . ?
P1 C13 1.803(3) . ?
P1 C7 1.812(3) . ?
P1 C1 1.818(3) . ?
P2 C19 1.802(3) . ?
P2 C26 1.815(3) . ?
P2 C20 1.816(3) . ?
N1 N2 1.353(3) . ?
N1 C13 1.372(3) . ?
N1 C16 1.460(3) . ?
N2 C15 1.330(3) . ?
N3 N4 1.353(3) . ?
N3 C19 1.370(3) . ?
N3 C16 1.448(3) . ?
N4 C17 1.334(4) . ?
C1 C2 1.394(4) . ?
C1 C6 1.395(4) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.396(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.380(4) . ?
C14 C15 1.404(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.397(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(4) . ?
C18 H18 0.9500 . ?
C20 C25 1.391(4) . ?
C20 C21 1.397(4) . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.390(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.393(4) . ?
C26 C31 1.394(4) . ?
C27 C28 1.392(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.382(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.382(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
C13 P1 C7 103.62(12) . . ?
C13 P1 C1 103.71(12) . . ?
C7 P1 C1 106.53(12) . . ?
C13 P1 Se1 114.84(9) . . ?
C7 P1 Se1 114.02(9) . . ?
C1 P1 Se1 113.07(9) . . ?
C19 P2 C26 102.55(12) . . ?
C19 P2 C20 105.40(13) . . ?
C26 P2 C20 108.97(13) . . ?
C19 P2 Se2 113.28(9) . . ?
C26 P2 Se2 112.69(9) . . ?
C20 P2 Se2 113.18(9) . . ?
N2 N1 C13 112.4(2) . . ?
N2 N1 C16 120.7(2) . . ?
C13 N1 C16 126.7(2) . . ?
C15 N2 N1 104.5(2) . . ?
N4 N3 C19 112.7(2) . . ?
N4 N3 C16 120.0(2) . . ?
C19 N3 C16 127.3(2) . . ?
C17 N4 N3 104.1(2) . . ?
C2 C1 C6 119.9(2) . . ?
C2 C1 P1 119.2(2) . . ?
C6 C1 P1 120.8(2) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.3(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C8 C7 C12 119.6(3) . . ?
C8 C7 P1 119.3(2) . . ?
C12 C7 P1 121.1(2) . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
N1 C13 C14 106.0(2) . . ?
N1 C13 P1 123.2(2) . . ?
C14 C13 P1 130.82(19) . . ?
C13 C14 C15 105.0(2) . . ?
C13 C14 H14 127.5 . . ?
C15 C14 H14 127.5 . . ?
N2 C15 C14 112.1(3) . . ?
N2 C15 H15 124.0 . . ?
C14 C15 H15 124.0 . . ?
N3 C16 N1 110.9(2) . . ?
N3 C16 H16A 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
N1 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
N4 C17 C18 112.2(3) . . ?
N4 C17 H17 123.9 . . ?
C18 C17 H17 123.9 . . ?
C19 C18 C17 105.2(2) . . ?
C19 C18 H18 127.4 . . ?
C17 C18 H18 127.4 . . ?
N3 C19 C18 105.8(2) . . ?
N3 C19 P2 124.4(2) . . ?
C18 C19 P2 129.8(2) . . ?
C25 C20 C21 119.6(3) . . ?
C25 C20 P2 119.0(2) . . ?
C21 C20 P2 121.4(2) . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.1(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C20 C25 C24 119.9(3) . . ?
C20 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C31 120.0(2) . . ?
C27 C26 P2 123.1(2) . . ?
C31 C26 P2 116.9(2) . . ?
C28 C27 C26 119.4(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 120.2(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 120.5(3) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C31 119.9(3) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C26 119.9(3) . . ?
C30 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?

_refine_diff_density_max         0.504
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_compound19_MSB592_0m
_database_code_depnum_ccdc_archive 'CCDC 1511162'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
Dichlorido(2-(diphenylphosphanyl)-1-{[2-(diphenylphosphanyl)-1H-imidazole]methyl}-1H-imidazole-κ²P,P')platinum(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 Cl2 N4 P2 Pt'
_chemical_formula_sum            'C31 H26 Cl2 N4 P2 Pt'
_chemical_formula_weight         782.49

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'
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'
Pt Pt -1.7033 8.3905 '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                   12.0662(8)
_cell_length_b                   18.1114(12)
_cell_length_c                   13.1999(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.314(1)
_cell_angle_gamma                90
_cell_volume                     2882.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9764
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      29.17

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   0.355
_exptl_transmission_factor_max   0.530
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    5.194
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.530
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 10 sec/frame.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50599
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.910
_diffrn_reflns_theta_max         29.205
_diffrn_reflns_theta_full        28.500
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7536
_reflns_number_gt                6741
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2008)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'

_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. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²+3.0269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7536
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0523
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Pt1 Pt 0.28617(2) 0.46559(2) 0.86648(2) 0.01263(3) Uani 1 1 d . . . . .
Cl1 Cl 0.21648(5) 0.43672(3) 1.02472(4) 0.01737(12) Uani 1 1 d . . . . .
Cl2 Cl 0.39396(6) 0.35658(4) 0.87373(5) 0.02350(13) Uani 1 1 d . . . . .
P1 P 0.22290(5) 0.58130(3) 0.87224(5) 0.01290(12) Uani 1 1 d . . . . .
P2 P 0.33911(5) 0.47405(3) 0.70585(5) 0.01444(12) Uani 1 1 d . . . . .
N1 N 0.31360(18) 0.71713(12) 0.83213(18) 0.0219(5) Uani 1 1 d . . . . .
N2 N 0.44616(17) 0.63196(12) 0.85122(16) 0.0167(4) Uani 1 1 d . . . . .
N3 N 0.54504(18) 0.53069(12) 0.77540(16) 0.0170(4) Uani 1 1 d . . . . .
N4 N 0.54936(19) 0.46952(12) 0.62915(17) 0.0210(5) Uani 1 1 d . . . . .
C1 C 0.10460(19) 0.59853(13) 0.78720(18) 0.0144(5) Uani 1 1 d . . . . .
C2 C 0.0307(2) 0.53935(13) 0.7762(2) 0.0173(5) Uani 1 1 d . . . . .
H2 H 0.0468 0.4939 0.8095 0.021 Uiso 1 1 calc R U . . .
C3 C -0.0660(2) 0.54692(15) 0.7169(2) 0.0208(5) Uani 1 1 d . . . . .
H3 H -0.1167 0.5069 0.7103 0.025 Uiso 1 1 calc R U . . .
C4 C -0.0889(2) 0.61312(15) 0.6670(2) 0.0223(6) Uani 1 1 d . . . . .
H4 H -0.1549 0.6183 0.6259 0.027 Uiso 1 1 calc R U . . .
C5 C -0.0153(2) 0.67151(15) 0.6775(2) 0.0236(6) Uani 1 1 d . . . . .
H5 H -0.0309 0.7164 0.6426 0.028 Uiso 1 1 calc R U . . .
C6 C 0.0811(2) 0.66544(14) 0.7382(2) 0.0197(5) Uani 1 1 d . . . . .
H6 H 0.1303 0.7062 0.7462 0.024 Uiso 1 1 calc R U . . .
C7 C 0.1793(2) 0.61090(13) 0.99584(18) 0.0159(5) Uani 1 1 d . . . . .
C8 C 0.0670(2) 0.61781(14) 1.0149(2) 0.0204(5) Uani 1 1 d . . . . .
H8 H 0.0128 0.6107 0.9616 0.024 Uiso 1 1 calc R U . . .
C9 C 0.0344(2) 0.63501(15) 1.1117(2) 0.0247(6) Uani 1 1 d . . . . .
H9 H -0.0421 0.6403 1.1242 0.030 Uiso 1 1 calc R U . . .
C10 C 0.1125(3) 0.64450(15) 1.1896(2) 0.0274(6) Uani 1 1 d . . . . .
H10 H 0.0897 0.6554 1.2560 0.033 Uiso 1 1 calc R U . . .
C11 C 0.2246(3) 0.63815(16) 1.1710(2) 0.0292(7) Uani 1 1 d . . . . .
H11 H 0.2785 0.6452 1.2246 0.035 Uiso 1 1 calc R U . . .
C12 C 0.2579(2) 0.62159(15) 1.0745(2) 0.0233(6) Uani 1 1 d . . . . .
H12 H 0.3346 0.6175 1.0619 0.028 Uiso 1 1 calc R U . . .
C13 C 0.3334(2) 0.64628(14) 0.84755(19) 0.0154(5) Uani 1 1 d . . . . .
C14 C 0.4160(2) 0.74973(15) 0.8237(2) 0.0265(6) Uani 1 1 d . . . . .
H14 H 0.4278 0.8007 0.8114 0.032 Uiso 1 1 calc R U . . .
C15 C 0.4973(2) 0.69853(15) 0.8355(2) 0.0249(6) Uani 1 1 d . . . . .
H15 H 0.5748 0.7070 0.8333 0.030 Uiso 1 1 calc R U . . .
C16 C 0.5086(2) 0.56418(14) 0.86925(19) 0.0171(5) Uani 1 1 d . . . . .
H16A H 0.4618 0.5284 0.9048 0.021 Uiso 1 1 calc R U . . .
H16B H 0.5744 0.5751 0.9140 0.021 Uiso 1 1 calc R U . . .
C17 C 0.6508(2) 0.53738(15) 0.7413(2) 0.0221(6) Uani 1 1 d . . . . .
H17 H 0.7111 0.5632 0.7733 0.026 Uiso 1 1 calc R U . . .
C18 C 0.6514(2) 0.49961(17) 0.6526(2) 0.0238(6) Uani 1 1 d . . . . .
H18 H 0.7143 0.4947 0.6121 0.029 Uiso 1 1 calc R U . . .
C19 C 0.4864(2) 0.48906(14) 0.70408(19) 0.0166(5) Uani 1 1 d . . . . .
C20 C 0.3045(2) 0.39014(14) 0.63580(19) 0.0181(5) Uani 1 1 d . . . . .
C21 C 0.3575(2) 0.37235(15) 0.5472(2) 0.0210(5) Uani 1 1 d . . . . .
H21 H 0.4156 0.4028 0.5244 0.025 Uiso 1 1 calc R U . . .
C22 C 0.3252(2) 0.31005(15) 0.4923(2) 0.0251(6) Uani 1 1 d . . . . .
H22 H 0.3619 0.2975 0.4323 0.030 Uiso 1 1 calc R U . . .
C23 C 0.2392(3) 0.26580(15) 0.5251(2) 0.0269(6) Uani 1 1 d . . . . .
H23 H 0.2178 0.2229 0.4878 0.032 Uiso 1 1 calc R U . . .
C24 C 0.1849(3) 0.28438(17) 0.6118(2) 0.0325(7) Uani 1 1 d . . . . .
H24 H 0.1250 0.2549 0.6331 0.039 Uiso 1 1 calc R U . . .
C25 C 0.2179(3) 0.34616(17) 0.6678(2) 0.0286(6) Uani 1 1 d . . . . .
H25 H 0.1813 0.3584 0.7279 0.034 Uiso 1 1 calc R U . . .
C26 C 0.2852(2) 0.54661(14) 0.62156(19) 0.0166(5) Uani 1 1 d . . . . .
C27 C 0.3441(2) 0.61162(14) 0.6069(2) 0.0202(5) Uani 1 1 d . . . . .
H27 H 0.4141 0.6187 0.6411 0.024 Uiso 1 1 calc R U . . .
C28 C 0.3012(3) 0.66616(16) 0.5428(2) 0.0263(6) Uani 1 1 d . . . . .
H28 H 0.3418 0.7104 0.5334 0.032 Uiso 1 1 calc R U . . .
C29 C 0.1991(3) 0.65623(17) 0.4921(2) 0.0287(6) Uani 1 1 d . . . . .
H29 H 0.1699 0.6936 0.4482 0.034 Uiso 1 1 calc R U . . .
C30 C 0.1400(2) 0.59154(16) 0.5058(2) 0.0240(6) Uani 1 1 d . . . . .
H30 H 0.0702 0.5847 0.4712 0.029 Uiso 1 1 calc R U . . .
C31 C 0.1825(2) 0.53673(14) 0.5702(2) 0.0193(5) Uani 1 1 d . . . . .
H31 H 0.1417 0.4925 0.5793 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 P1 2.2327(6) . ?
Pt1 P2 2.2442(7) . ?
Pt1 Cl1 2.3420(6) . ?
Pt1 Cl2 2.3641(6) . ?
P1 C1 1.807(2) . ?
P1 C7 1.815(3) . ?
P1 C13 1.817(3) . ?
P2 C19 1.799(3) . ?
P2 C20 1.819(3) . ?
P2 C26 1.825(3) . ?
N1 C13 1.320(3) . ?
N1 C14 1.378(3) . ?
N2 C15 1.374(3) . ?
N2 C13 1.384(3) . ?
N2 C16 1.455(3) . ?
N3 C17 1.376(3) . ?
N3 C19 1.379(3) . ?
N3 C16 1.463(3) . ?
N4 C19 1.320(3) . ?
N4 C18 1.371(4) . ?
C1 C6 1.397(3) . ?
C1 C2 1.398(3) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.391(4) . ?
C7 C8 1.394(4) . ?
C8 C9 1.387(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.354(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.356(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C20 C25 1.393(4) . ?
C20 C21 1.393(4) . ?
C21 C22 1.388(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.393(4) . ?
C26 C31 1.400(4) . ?
C27 C28 1.388(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
P1 Pt1 P2 94.53(2) . . ?
P1 Pt1 Cl1 92.50(2) . . ?
P2 Pt1 Cl1 169.73(2) . . ?
P1 Pt1 Cl2 166.13(2) . . ?
P2 Pt1 Cl2 85.30(2) . . ?
Cl1 Pt1 Cl2 89.67(2) . . ?
C1 P1 C7 104.89(11) . . ?
C1 P1 C13 110.09(11) . . ?
C7 P1 C13 102.19(11) . . ?
C1 P1 Pt1 113.80(8) . . ?
C7 P1 Pt1 114.82(8) . . ?
C13 P1 Pt1 110.33(8) . . ?
C19 P2 C20 109.06(12) . . ?
C19 P2 C26 102.19(12) . . ?
C20 P2 C26 102.88(12) . . ?
C19 P2 Pt1 109.97(9) . . ?
C20 P2 Pt1 110.80(9) . . ?
C26 P2 Pt1 121.14(8) . . ?
C13 N1 C14 105.8(2) . . ?
C15 N2 C13 106.1(2) . . ?
C15 N2 C16 122.2(2) . . ?
C13 N2 C16 131.7(2) . . ?
C17 N3 C19 106.4(2) . . ?
C17 N3 C16 123.7(2) . . ?
C19 N3 C16 129.9(2) . . ?
C19 N4 C18 105.3(2) . . ?
C6 C1 C2 120.0(2) . . ?
C6 C1 P1 125.29(19) . . ?
C2 C1 P1 114.61(18) . . ?
C3 C2 C1 120.1(2) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.0(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.0(2) . . ?
C5 C6 H6 120.5 . . ?
C1 C6 H6 120.5 . . ?
C12 C7 C8 119.4(2) . . ?
C12 C7 P1 119.9(2) . . ?
C8 C7 P1 120.52(19) . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 119.9(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 N2 111.0(2) . . ?
N1 C13 P1 121.87(19) . . ?
N2 C13 P1 126.84(19) . . ?
C15 C14 N1 110.2(2) . . ?
C15 C14 H14 124.9 . . ?
N1 C14 H14 124.9 . . ?
C14 C15 N2 106.9(2) . . ?
C14 C15 H15 126.5 . . ?
N2 C15 H15 126.5 . . ?
N2 C16 N3 112.5(2) . . ?
N2 C16 H16A 109.1 . . ?
N3 C16 H16A 109.1 . . ?
N2 C16 H16B 109.1 . . ?
N3 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 N3 106.0(2) . . ?
C18 C17 H17 127.0 . . ?
N3 C17 H17 127.0 . . ?
C17 C18 N4 111.1(2) . . ?
C17 C18 H18 124.5 . . ?
N4 C18 H18 124.5 . . ?
N4 C19 N3 111.3(2) . . ?
N4 C19 P2 124.6(2) . . ?
N3 C19 P2 123.63(19) . . ?
C25 C20 C21 119.8(2) . . ?
C25 C20 P2 118.9(2) . . ?
C21 C20 P2 121.1(2) . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 120.1(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 120.0(3) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 120.1(3) . . ?
C24 C25 H25 119.9 . . ?
C20 C25 H25 119.9 . . ?
C27 C26 C31 119.2(2) . . ?
C27 C26 P2 121.5(2) . . ?
C31 C26 P2 119.3(2) . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 120.2(3) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.2(3) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C26 120.1(3) . . ?
C30 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?

_refine_diff_density_max         2.042
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_compound23_MSB695_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1511163'
_audit_update_record             
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H36 N4 P2 Pd2, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C38 H38 B2 Cl2 F8 N4 P2 Pd2'
_chemical_formula_weight         1069.98

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'
B B 0.0013 0.0007 '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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.1418(5)
_cell_length_b                   31.8019(15)
_cell_length_c                   11.9253(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.2500(7)
_cell_angle_gamma                90
_cell_volume                     4129.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9707
_cell_measurement_theta_min      2.362
_cell_measurement_theta_max      29.118

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale gold'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   0.602
_exptl_transmission_factor_max   0.794
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.149
_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.92

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            76153
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.861
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_full        28.500
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10965
_reflns_number_gt                9158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 - 0.99 Å). 
All were included as riding contributions with isotropic displacement 
parameters 1.2 - 1.5 times those of the attached atoms. Both allyl groups 
and one tetrafluoroborate anion are disordered over two resolved orientations. 
The disorder was modeled by restraining the two components of each disordered 
group to have comparable geometries.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+8.6289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10965
_refine_ls_number_parameters     553
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.005
_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
Pd1 Pd 0.65473(2) 0.61622(2) 0.11590(2) 0.01583(5) Uani 1 1 d D . . . .
Pd2 Pd 0.31348(2) 0.70824(2) 0.42554(2) 0.01716(6) Uani 1 1 d D . . . .
P1 P 0.52415(6) 0.57378(2) 0.18969(6) 0.01614(13) Uani 1 1 d . . . . .
P2 P 0.44121(6) 0.75279(2) 0.34995(6) 0.01602(13) Uani 1 1 d . . . . .
N1 N 0.4203(2) 0.63791(7) 0.29379(18) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.3910(2) 0.65102(7) 0.39301(19) 0.0179(4) Uani 1 1 d . . . . .
N3 N 0.5381(2) 0.69103(7) 0.22844(19) 0.0146(4) Uani 1 1 d . . . . .
N4 N 0.6435(2) 0.67341(7) 0.20905(19) 0.0159(4) Uani 1 1 d . . . . .
C1 C 0.3778(2) 0.55765(8) 0.1010(2) 0.0189(5) Uani 1 1 d . . . . .
C2 C 0.3616(3) 0.55755(9) -0.0180(3) 0.0243(6) Uani 1 1 d . . . . .
H2 H 0.4258 0.5668 -0.0532 0.029 Uiso 1 1 calc R U . . .
C3 C 0.2508(3) 0.54378(10) -0.0852(3) 0.0305(7) Uani 1 1 d . . . . .
H3 H 0.2397 0.5435 -0.1664 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1573(3) 0.53053(10) -0.0343(3) 0.0309(7) Uani 1 1 d . . . . .
H4 H 0.0826 0.5206 -0.0806 0.037 Uiso 1 1 calc R U . . .
C5 C 0.1715(3) 0.53161(10) 0.0837(3) 0.0299(7) Uani 1 1 d . . . . .
H5 H 0.1062 0.5230 0.1183 0.036 Uiso 1 1 calc R U . . .
C6 C 0.2813(3) 0.54530(9) 0.1514(3) 0.0245(6) Uani 1 1 d . . . . .
H6 H 0.2909 0.5463 0.2324 0.029 Uiso 1 1 calc R U . . .
C7 C 0.5969(2) 0.52703(8) 0.2607(2) 0.0181(5) Uani 1 1 d . . . . .
C8 C 0.5363(3) 0.48853(9) 0.2565(2) 0.0220(6) Uani 1 1 d . . . . .
H8 H 0.4546 0.4858 0.2132 0.026 Uiso 1 1 calc R U . . .
C9 C 0.5952(3) 0.45423(10) 0.3154(3) 0.0288(7) Uani 1 1 d . . . . .
H9 H 0.5542 0.4279 0.3117 0.035 Uiso 1 1 calc R U . . .
C10 C 0.7139(3) 0.45819(10) 0.3799(3) 0.0295(7) Uani 1 1 d . . . . .
H10 H 0.7533 0.4348 0.4216 0.035 Uiso 1 1 calc R U . . .
C11 C 0.7751(3) 0.49614(10) 0.3835(3) 0.0275(6) Uani 1 1 d . . . . .
H11 H 0.8566 0.4987 0.4273 0.033 Uiso 1 1 calc R U . . .
C12 C 0.7175(3) 0.53048(9) 0.3231(3) 0.0243(6) Uani 1 1 d . . . . .
H12 H 0.7602 0.5564 0.3244 0.029 Uiso 1 1 calc R U . . .
C13 C 0.4730(2) 0.59898(8) 0.3075(2) 0.0177(5) Uani 1 1 d . . . . .
C14 C 0.4737(3) 0.58627(9) 0.4178(2) 0.0226(6) Uani 1 1 d . . . . .
H14 H 0.5032 0.5604 0.4529 0.027 Uiso 1 1 calc R U . . .
C15 C 0.4215(3) 0.61964(9) 0.4671(2) 0.0230(6) Uani 1 1 d . . . . .
H15 H 0.4094 0.6199 0.5436 0.028 Uiso 1 1 calc R U . . .
C16 C 0.4243(2) 0.66773(8) 0.2025(2) 0.0152(5) Uani 1 1 d . . . . .
H16A H 0.4178 0.6525 0.1289 0.018 Uiso 1 1 calc R U . . .
H16B H 0.3541 0.6874 0.1942 0.018 Uiso 1 1 calc R U . . .
C17 C 0.7338(2) 0.69810(9) 0.2630(2) 0.0192(5) Uani 1 1 d . . . . .
H17 H 0.8183 0.6939 0.2633 0.023 Uiso 1 1 calc R U . . .
C18 C 0.6881(2) 0.73128(9) 0.3196(2) 0.0190(5) Uani 1 1 d . . . . .
H18 H 0.7340 0.7531 0.3636 0.023 Uiso 1 1 calc R U . . .
C19 C 0.5626(2) 0.72557(8) 0.2977(2) 0.0157(5) Uani 1 1 d . . . . .
C20 C 0.3674(2) 0.78507(8) 0.2294(2) 0.0182(5) Uani 1 1 d . . . . .
C21 C 0.4288(3) 0.79857(11) 0.1456(3) 0.0295(7) Uani 1 1 d . . . . .
H21 H 0.5104 0.7894 0.1478 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3713(3) 0.82530(12) 0.0588(3) 0.0350(8) Uani 1 1 d . . . . .
H22 H 0.4136 0.8343 0.0018 0.042 Uiso 1 1 calc R U . . .
C23 C 0.2522(3) 0.83892(11) 0.0550(3) 0.0315(7) Uani 1 1 d . . . . .
H23 H 0.2132 0.8574 -0.0042 0.038 Uiso 1 1 calc R U . . .
C24 C 0.1908(3) 0.82551(11) 0.1375(3) 0.0341(7) Uani 1 1 d . . . . .
H24 H 0.1093 0.8348 0.1350 0.041 Uiso 1 1 calc R U . . .
C25 C 0.2477(3) 0.79858(10) 0.2239(3) 0.0277(6) Uani 1 1 d . . . . .
H25 H 0.2045 0.7893 0.2800 0.033 Uiso 1 1 calc R U . . .
C26 C 0.5250(2) 0.78855(8) 0.4565(2) 0.0179(5) Uani 1 1 d . . . . .
C27 C 0.5318(3) 0.77945(10) 0.5723(2) 0.0232(6) Uani 1 1 d . . . . .
H27 H 0.5015 0.7534 0.5939 0.028 Uiso 1 1 calc R U . . .
C28 C 0.5827(3) 0.80852(11) 0.6557(3) 0.0311(7) Uani 1 1 d . . . . .
H28 H 0.5862 0.8025 0.7344 0.037 Uiso 1 1 calc R U . . .
C29 C 0.6284(3) 0.84630(10) 0.6248(3) 0.0297(7) Uani 1 1 d . . . . .
H29 H 0.6608 0.8665 0.6819 0.036 Uiso 1 1 calc R U . . .
C30 C 0.6267(3) 0.85458(10) 0.5118(3) 0.0296(7) Uani 1 1 d . . . . .
H30 H 0.6612 0.8800 0.4913 0.036 Uiso 1 1 calc R U . . .
C31 C 0.5749(3) 0.82606(9) 0.4265(3) 0.0237(6) Uani 1 1 d . . . . .
H31 H 0.5736 0.8321 0.3483 0.028 Uiso 1 1 calc R U . . .
C32 C 0.6888(8) 0.5702(3) -0.0027(7) 0.0276(17) Uani 0.566(6) 1 d D . P A 1
H32A H 0.6164 0.5844 -0.0403 0.033 Uiso 0.566(6) 1 calc R U P A 1
H32B H 0.6874 0.5407 0.0089 0.033 Uiso 0.566(6) 1 calc R U P A 1
C33 C 0.7975(5) 0.59281(17) 0.0355(5) 0.0278(9) Uani 0.566(6) 1 d D . P A 1
H33 H 0.8711 0.5794 0.0733 0.033 Uiso 0.566(6) 1 calc R U P A 1
C34 C 0.7925(10) 0.6358(4) 0.0155(10) 0.026(2) Uani 0.566(6) 1 d D . P A 1
H34A H 0.7177 0.6485 -0.0225 0.032 Uiso 0.566(6) 1 calc R U P A 1
H34B H 0.8639 0.6526 0.0398 0.032 Uiso 0.566(6) 1 calc R U P A 1
C32A C 0.7179(12) 0.5646(3) 0.0331(9) 0.0276(17) Uani 0.434(6) 1 d D . P A 2
H32C H 0.7507 0.5612 0.1129 0.033 Uiso 0.434(6) 1 calc R U P A 2
H32D H 0.6685 0.5430 -0.0085 0.033 Uiso 0.434(6) 1 calc R U P A 2
C33A C 0.7426(7) 0.6015(2) -0.0237(7) 0.0278(9) Uani 0.434(6) 1 d D . P A 2
H33A H 0.7104 0.6052 -0.1034 0.033 Uiso 0.434(6) 1 calc R U P A 2
C34A C 0.8152(13) 0.6322(5) 0.0401(15) 0.026(2) Uani 0.434(6) 1 d D . P A 2
H34C H 0.8468 0.6281 0.1198 0.032 Uiso 0.434(6) 1 calc R U P A 2
H34D H 0.8332 0.6574 0.0040 0.032 Uiso 0.434(6) 1 calc R U P A 2
C35 C 0.1788(18) 0.6806(3) 0.5138(18) 0.0288(12) Uani 0.619(6) 1 d D . P B 1
H35A H 0.2599 0.6760 0.5563 0.035 Uiso 0.619(6) 1 calc R U P B 1
H35B H 0.1233 0.6577 0.4959 0.035 Uiso 0.619(6) 1 calc R U P B 1
C36 C 0.1418(4) 0.72028(16) 0.4782(4) 0.0262(9) Uani 0.619(6) 1 d D . P B 1
H36 H 0.0602 0.7241 0.4357 0.031 Uiso 0.619(6) 1 calc R U P B 1
C37 C 0.2164(18) 0.7545(3) 0.5007(17) 0.0373(19) Uani 0.619(6) 1 d D . P B 1
H37A H 0.2983 0.7514 0.5431 0.045 Uiso 0.619(6) 1 calc R U P B 1
H37B H 0.1865 0.7815 0.4742 0.045 Uiso 0.619(6) 1 calc R U P B 1
C35A C 0.186(3) 0.6768(5) 0.516(3) 0.0288(12) Uani 0.381(6) 1 d D . P B 2
H35C H 0.1615 0.6720 0.4358 0.035 Uiso 0.381(6) 1 calc R U P B 2
H35D H 0.1934 0.6539 0.5680 0.035 Uiso 0.381(6) 1 calc R U P B 2
C36A C 0.2098(7) 0.7166(3) 0.5564(7) 0.0262(9) Uani 0.381(6) 1 d D . P B 2
H36A H 0.2338 0.7198 0.6373 0.031 Uiso 0.381(6) 1 calc R U P B 2
C37A C 0.203(3) 0.7523(5) 0.492(3) 0.0373(19) Uani 0.381(6) 1 d D . P B 2
H37C H 0.1791 0.7507 0.4111 0.045 Uiso 0.381(6) 1 calc R U P B 2
H37D H 0.2214 0.7787 0.5289 0.045 Uiso 0.381(6) 1 calc R U P B 2
B1 B 0.0257(3) 0.58175(13) 0.3474(3) 0.0303(8) Uani 1 1 d . . . . .
F1 F 0.14817(19) 0.59196(7) 0.35614(19) 0.0439(5) Uani 1 1 d . . . . .
F2 F -0.0100(2) 0.55189(9) 0.2634(2) 0.0612(7) Uani 1 1 d . . . . .
F3 F 0.0088(2) 0.56644(10) 0.4511(2) 0.0660(8) Uani 1 1 d . . . . .
F4 F -0.0455(2) 0.61729(8) 0.3196(2) 0.0629(7) Uani 1 1 d . . . . .
B2 B 0.4296(3) 0.67776(14) 0.8300(3) 0.0368(9) Uani 1 1 d D . . . .
F5 F 0.5035(6) 0.64735(16) 0.8041(6) 0.120(3) Uani 0.702(4) 1 d D . P C 1
F6 F 0.3106(4) 0.66573(16) 0.7894(4) 0.0876(16) Uani 0.702(4) 1 d D . P C 1
F7 F 0.4433(6) 0.68019(18) 0.9462(3) 0.1012(18) Uani 0.702(4) 1 d D . P C 1
F5A F 0.3902(11) 0.6524(3) 0.7390(9) 0.120(3) Uani 0.298(4) 1 d D . P C 2
F6A F 0.3588(8) 0.6813(3) 0.9032(9) 0.0876(16) Uani 0.298(4) 1 d D . P C 2
F7A F 0.5462(9) 0.6655(4) 0.8834(8) 0.1012(18) Uani 0.298(4) 1 d D . P C 2
F8 F 0.4507(2) 0.71637(8) 0.7840(2) 0.0597(7) Uani 1 1 d D . . . .
C38 C 0.8762(4) 0.55197(15) 0.6551(4) 0.0494(10) Uani 1 1 d . . . . .
H38A H 0.9181 0.5244 0.6667 0.059 Uiso 1 1 calc R U . . .
H38B H 0.8875 0.5636 0.5811 0.059 Uiso 1 1 calc R U . . .
Cl1 Cl 0.71896(10) 0.54524(4) 0.65082(11) 0.0621(3) Uani 1 1 d . . . . .
Cl2 Cl 0.94156(14) 0.58607(4) 0.76662(12) 0.0806(4) 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
Pd1 C32A 2.113(10) . ?
Pd1 C32 2.124(8) . ?
Pd1 N4 2.148(2) . ?
Pd1 C33A 2.154(6) . ?
Pd1 C33 2.157(5) . ?
Pd1 C34 2.227(9) . ?
Pd1 C34A 2.227(12) . ?
Pd1 P1 2.2927(7) . ?
Pd2 N2 2.086(2) . ?
Pd2 C37A 2.130(13) . ?
Pd2 C37 2.133(8) . ?
Pd2 C36A 2.147(7) . ?
Pd2 C36 2.170(4) . ?
Pd2 C35 2.191(8) . ?
Pd2 C35A 2.199(13) . ?
Pd2 P2 2.3215(7) . ?
P1 C13 1.811(3) . ?
P1 C7 1.815(3) . ?
P1 C1 1.819(3) . ?
P2 C26 1.810(3) . ?
P2 C20 1.815(3) . ?
P2 C19 1.824(3) . ?
N1 N2 1.358(3) . ?
N1 C13 1.365(3) . ?
N1 C16 1.452(3) . ?
N2 C15 1.328(4) . ?
N3 N4 1.365(3) . ?
N3 C19 1.367(3) . ?
N3 C16 1.444(3) . ?
N4 C17 1.330(3) . ?
C1 C2 1.392(4) . ?
C1 C6 1.395(4) . ?
C2 C3 1.392(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.394(4) . ?
C7 C12 1.395(4) . ?
C8 C9 1.386(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.375(4) . ?
C14 C15 1.398(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.405(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(4) . ?
C18 H18 0.9500 . ?
C20 C25 1.390(4) . ?
C20 C21 1.393(4) . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.386(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.394(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.388(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.369(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.393(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.398(9) . ?
C32 H32A 0.9500 . ?
C32 H32B 0.9500 . ?
C33 C34 1.387(11) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C32A C33A 1.412(11) . ?
C32A H32C 0.9500 . ?
C32A H32D 0.9500 . ?
C33A C34A 1.388(13) . ?
C33A H33A 0.9500 . ?
C34A H34C 0.9500 . ?
C34A H34D 0.9500 . ?
C35 C36 1.366(14) . ?
C35 H35A 0.9500 . ?
C35 H35B 0.9500 . ?
C36 C37 1.362(15) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9500 . ?
C37 H37B 0.9500 . ?
C35A C36A 1.359(17) . ?
C35A H35C 0.9500 . ?
C35A H35D 0.9500 . ?
C36A C37A 1.361(17) . ?
C36A H36A 0.9500 . ?
C37A H37C 0.9500 . ?
C37A H37D 0.9500 . ?
B1 F2 1.377(5) . ?
B1 F3 1.379(4) . ?
B1 F4 1.380(5) . ?
B1 F1 1.385(4) . ?
B2 F6A 1.301(8) . ?
B2 F5 1.347(6) . ?
B2 F5A 1.348(9) . ?
B2 F7 1.364(5) . ?
B2 F6 1.366(5) . ?
B2 F7A 1.376(9) . ?
B2 F8 1.385(5) . ?
C38 Cl2 1.750(4) . ?
C38 Cl1 1.755(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C32A Pd1 N4 164.0(4) . . ?
C32 Pd1 N4 164.9(3) . . ?
C32A Pd1 C33A 38.6(3) . . ?
N4 Pd1 C33A 132.0(2) . . ?
C32 Pd1 C33 38.1(3) . . ?
N4 Pd1 C33 130.64(16) . . ?
C32 Pd1 C34 66.0(4) . . ?
N4 Pd1 C34 99.4(3) . . ?
C33 Pd1 C34 36.8(3) . . ?
C32A Pd1 C34A 67.2(5) . . ?
N4 Pd1 C34A 99.0(4) . . ?
C33A Pd1 C34A 36.9(4) . . ?
C32A Pd1 P1 91.3(3) . . ?
C32 Pd1 P1 93.9(3) . . ?
N4 Pd1 P1 100.88(6) . . ?
C33A Pd1 P1 126.8(2) . . ?
C33 Pd1 P1 123.73(15) . . ?
C34 Pd1 P1 159.6(3) . . ?
C34A Pd1 P1 156.9(4) . . ?
N2 Pd2 C37A 159.9(5) . . ?
N2 Pd2 C37 161.3(3) . . ?
N2 Pd2 C36A 123.4(2) . . ?
C37A Pd2 C36A 37.1(5) . . ?
N2 Pd2 C36 129.27(15) . . ?
C37 Pd2 C36 36.9(4) . . ?
N2 Pd2 C35 95.3(3) . . ?
C37 Pd2 C35 67.3(4) . . ?
C36 Pd2 C35 36.5(4) . . ?
N2 Pd2 C35A 91.8(5) . . ?
C37A Pd2 C35A 68.2(7) . . ?
C36A Pd2 C35A 36.4(5) . . ?
N2 Pd2 P2 98.50(6) . . ?
C37A Pd2 P2 101.3(5) . . ?
C37 Pd2 P2 98.6(3) . . ?
C36A Pd2 P2 132.5(2) . . ?
C36 Pd2 P2 130.95(14) . . ?
C35 Pd2 P2 165.9(3) . . ?
C35A Pd2 P2 168.9(5) . . ?
C13 P1 C7 100.60(12) . . ?
C13 P1 C1 100.65(13) . . ?
C7 P1 C1 107.28(12) . . ?
C13 P1 Pd1 111.52(9) . . ?
C7 P1 Pd1 113.84(9) . . ?
C1 P1 Pd1 120.43(9) . . ?
C26 P2 C20 106.27(12) . . ?
C26 P2 C19 103.21(12) . . ?
C20 P2 C19 104.00(12) . . ?
C26 P2 Pd2 112.22(9) . . ?
C20 P2 Pd2 116.16(9) . . ?
C19 P2 Pd2 113.79(9) . . ?
N2 N1 C13 110.6(2) . . ?
N2 N1 C16 120.3(2) . . ?
C13 N1 C16 127.0(2) . . ?
C15 N2 N1 105.9(2) . . ?
C15 N2 Pd2 126.08(19) . . ?
N1 N2 Pd2 127.99(17) . . ?
N4 N3 C19 111.3(2) . . ?
N4 N3 C16 120.1(2) . . ?
C19 N3 C16 126.6(2) . . ?
C17 N4 N3 105.4(2) . . ?
C17 N4 Pd1 128.99(18) . . ?
N3 N4 Pd1 125.57(16) . . ?
C2 C1 C6 119.6(3) . . ?
C2 C1 P1 120.0(2) . . ?
C6 C1 P1 120.5(2) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C8 C7 C12 119.5(3) . . ?
C8 C7 P1 122.5(2) . . ?
C12 C7 P1 118.0(2) . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.2(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C7 120.1(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 C14 107.2(2) . . ?
N1 C13 P1 120.5(2) . . ?
C14 C13 P1 132.3(2) . . ?
C13 C14 C15 105.1(2) . . ?
C13 C14 H14 127.4 . . ?
C15 C14 H14 127.4 . . ?
N2 C15 C14 111.1(2) . . ?
N2 C15 H15 124.4 . . ?
C14 C15 H15 124.4 . . ?
N3 C16 N1 109.8(2) . . ?
N3 C16 H16A 109.7 . . ?
N1 C16 H16A 109.7 . . ?
N3 C16 H16B 109.7 . . ?
N1 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N4 C17 C18 111.2(2) . . ?
N4 C17 H17 124.4 . . ?
C18 C17 H17 124.4 . . ?
C19 C18 C17 105.5(2) . . ?
C19 C18 H18 127.3 . . ?
C17 C18 H18 127.3 . . ?
N3 C19 C18 106.5(2) . . ?
N3 C19 P2 121.36(19) . . ?
C18 C19 P2 132.0(2) . . ?
C25 C20 C21 118.9(3) . . ?
C25 C20 P2 118.7(2) . . ?
C21 C20 P2 122.3(2) . . ?
C22 C21 C20 120.3(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 120.2(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 120.6(3) . . ?
C24 C25 H25 119.7 . . ?
C20 C25 H25 119.7 . . ?
C31 C26 C27 119.3(3) . . ?
C31 C26 P2 122.1(2) . . ?
C27 C26 P2 118.4(2) . . ?
C28 C27 C26 119.9(3) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 120.3(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C30 C29 C28 120.0(3) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.7(3) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C26 119.7(3) . . ?
C30 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C33 C32 Pd1 72.2(4) . . ?
C33 C32 H32A 120.0 . . ?
Pd1 C32 H32A 74.5 . . ?
C33 C32 H32B 120.0 . . ?
Pd1 C32 H32B 124.9 . . ?
H32A C32 H32B 120.0 . . ?
C34 C33 C32 116.7(8) . . ?
C34 C33 Pd1 74.3(4) . . ?
C32 C33 Pd1 69.7(4) . . ?
C34 C33 H33 121.6 . . ?
C32 C33 H33 121.6 . . ?
Pd1 C33 H33 126.1 . . ?
C33 C34 Pd1 68.8(4) . . ?
C33 C34 H34A 120.0 . . ?
Pd1 C34 H34A 74.9 . . ?
C33 C34 H34B 120.0 . . ?
Pd1 C34 H34B 128.4 . . ?
H34A C34 H34B 120.0 . . ?
C33A C32A Pd1 72.2(5) . . ?
C33A C32A H32C 120.0 . . ?
Pd1 C32A H32C 73.4 . . ?
C33A C32A H32D 120.0 . . ?
Pd1 C32A H32D 126.2 . . ?
H32C C32A H32D 120.0 . . ?
C34A C33A C32A 118.3(11) . . ?
C34A C33A Pd1 74.4(6) . . ?
C32A C33A Pd1 69.1(5) . . ?
C34A C33A H33A 120.9 . . ?
C32A C33A H33A 120.9 . . ?
Pd1 C33A H33A 127.5 . . ?
C33A C34A Pd1 68.7(5) . . ?
C33A C34A H34C 120.0 . . ?
Pd1 C34A H34C 73.8 . . ?
C33A C34A H34D 120.0 . . ?
Pd1 C34A H34D 129.9 . . ?
H34C C34A H34D 120.0 . . ?
C36 C35 Pd2 70.9(4) . . ?
C36 C35 H35A 120.0 . . ?
Pd2 C35 H35A 69.4 . . ?
C36 C35 H35B 120.0 . . ?
Pd2 C35 H35B 132.8 . . ?
H35A C35 H35B 120.0 . . ?
C37 C36 C35 123.1(14) . . ?
C37 C36 Pd2 70.1(4) . . ?
C35 C36 Pd2 72.6(5) . . ?
C37 C36 H36 118.5 . . ?
C35 C36 H36 118.5 . . ?
Pd2 C36 H36 132.2 . . ?
C36 C37 Pd2 73.0(4) . . ?
C36 C37 H37A 120.0 . . ?
Pd2 C37 H37A 68.7 . . ?
C36 C37 H37B 120.0 . . ?
Pd2 C37 H37B 131.0 . . ?
H37A C37 H37B 120.0 . . ?
C36A C35A Pd2 69.7(6) . . ?
C36A C35A H35C 120.0 . . ?
Pd2 C35A H35C 69.8 . . ?
C36A C35A H35D 120.0 . . ?
Pd2 C35A H35D 133.8 . . ?
H35C C35A H35D 120.0 . . ?
C35A C36A C37A 126(2) . . ?
C35A C36A Pd2 73.9(7) . . ?
C37A C36A Pd2 70.8(7) . . ?
C35A C36A H36A 116.8 . . ?
C37A C36A H36A 116.8 . . ?
Pd2 C36A H36A 132.2 . . ?
C36A C37A Pd2 72.1(6) . . ?
C36A C37A H37C 120.0 . . ?
Pd2 C37A H37C 69.0 . . ?
C36A C37A H37D 120.0 . . ?
Pd2 C37A H37D 131.7 . . ?
H37C C37A H37D 120.0 . . ?
F2 B1 F3 109.6(3) . . ?
F2 B1 F4 109.1(3) . . ?
F3 B1 F4 108.9(3) . . ?
F2 B1 F1 110.1(3) . . ?
F3 B1 F1 109.6(3) . . ?
F4 B1 F1 109.5(3) . . ?
F6A B2 F5A 116.8(7) . . ?
F5 B2 F7 109.3(5) . . ?
F5 B2 F6 108.2(5) . . ?
F7 B2 F6 105.5(4) . . ?
F6A B2 F7A 111.2(6) . . ?
F5A B2 F7A 108.5(7) . . ?
F6A B2 F8 111.5(6) . . ?
F5 B2 F8 112.5(4) . . ?
F5A B2 F8 105.4(5) . . ?
F7 B2 F8 111.1(4) . . ?
F6 B2 F8 110.0(3) . . ?
F7A B2 F8 102.2(5) . . ?
Cl2 C38 Cl1 110.5(2) . . ?
Cl2 C38 H38A 109.6 . . ?
Cl1 C38 H38A 109.6 . . ?
Cl2 C38 H38B 109.6 . . ?
Cl1 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?

_refine_diff_density_max         1.436
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.105

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Compound-11
_database_code_depnum_ccdc_archive 'CCDC 1517753'
_audit_update_record             
;
2016-11-17 deposited with the CCDC.
2016-11-23 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         'C36 H31 Cl N4 P2 Ru'
_chemical_formula_sum            'C36 H31 Cl N4 P2 Ru'
_chemical_formula_weight         718.11

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'
N N 0.0061 0.0033 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1612(3)
_cell_length_b                   12.9584(5)
_cell_length_c                   15.8185(3)
_cell_angle_alpha                98.610(2)
_cell_angle_beta                 92.840(2)
_cell_angle_gamma                107.317(3)
_cell_volume                     1763.73(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12626
_cell_measurement_theta_min      1.9740
_cell_measurement_theta_max      31.0190

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.145
_exptl_absorpt_coefficient_mu    0.641
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.77653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'NUMABS RIGAKU 199'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku saturn 724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            14246
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.725
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6160
_reflns_number_gt                5664
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0554P)²+3.3901P] 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         6160
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1051
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.29716(3) 0.26278(2) 0.81897(2) 0.01391(9) Uani 1 1 d . . . . .
Cl1 Cl 0.04647(9) 0.22812(7) 0.87716(5) 0.02189(18) Uani 1 1 d . . . . .
P2 P 0.32900(9) 0.43446(6) 0.78472(5) 0.01413(17) Uani 1 1 d . . . . .
P1 P 0.17419(9) 0.16815(6) 0.68796(5) 0.01388(17) Uani 1 1 d . . . . .
N1 N -0.0968(3) 0.2310(2) 0.67565(17) 0.0174(6) Uani 1 1 d . . . . .
N3 N 0.0809(3) 0.4066(2) 0.66485(17) 0.0169(5) Uani 1 1 d . . . . .
N2 N -0.2513(3) 0.1938(2) 0.65228(19) 0.0246(6) Uani 1 1 d . . . . .
N4 N 0.0310(3) 0.4322(2) 0.59058(18) 0.0236(6) Uani 1 1 d . . . . .
C33 C 0.7813(4) 0.6090(3) 0.8574(3) 0.0275(8) Uani 1 1 d . . . . .
H33 H 0.8388 0.6476 0.9086 0.033 Uiso 1 1 calc R U . . .
C32 C 0.6223(4) 0.5675(3) 0.8540(2) 0.0224(7) Uani 1 1 d . . . . .
H32 H 0.5743 0.5802 0.9032 0.027 Uiso 1 1 calc R U . . .
C22 C 0.2371(4) 0.4498(3) 0.68398(19) 0.0162(6) Uani 1 1 d . . . . .
C6 C 0.2550(4) 0.2102(3) 0.5905(2) 0.0170(6) Uani 1 1 d . . . . .
C18 C -0.0304(4) 0.1489(3) 0.66355(19) 0.0165(6) Uani 1 1 d . . . . .
C12 C 0.1661(4) 0.0229(3) 0.6735(2) 0.0189(7) Uani 1 1 d . . . . .
C23 C 0.2890(4) 0.5063(3) 0.6179(2) 0.0214(7) Uani 1 1 d . . . . .
H23 H 0.3898 0.5454 0.6115 0.026 Uiso 1 1 calc R U . . .
C25 C 0.2753(4) 0.5403(3) 0.8563(2) 0.0175(6) Uani 1 1 d . . . . .
C7 C 0.4133(4) 0.2336(3) 0.5876(2) 0.0233(7) Uani 1 1 d . . . . .
H7 H 0.4745 0.2312 0.6356 0.028 Uiso 1 1 calc R U . . .
C24 C 0.1581(4) 0.4920(3) 0.5631(2) 0.0249(7) Uani 1 1 d . . . . .
H24 H 0.1596 0.5212 0.5127 0.030 Uiso 1 1 calc R U . . .
C31 C 0.5331(4) 0.5075(3) 0.7787(2) 0.0173(6) Uani 1 1 d . . . . .
C19 C -0.1473(4) 0.0549(3) 0.6308(2) 0.0226(7) Uani 1 1 d . . . . .
H19 H -0.1401 -0.0154 0.6154 0.027 Uiso 1 1 calc R U . . .
C36 C 0.6069(4) 0.4917(3) 0.7049(2) 0.0218(7) Uani 1 1 d . . . . .
H36 H 0.5500 0.4514 0.6539 0.026 Uiso 1 1 calc R U . . .
C27 C 0.1619(4) 0.5973(3) 0.9821(2) 0.0257(8) Uani 1 1 d . . . . .
H27 H 0.1120 0.5808 1.0304 0.031 Uiso 1 1 calc R U . . .
C16 C 0.1011(5) -0.1445(3) 0.7319(3) 0.0330(9) Uani 1 1 d . . . . .
H16 H 0.0605 -0.1834 0.7747 0.040 Uiso 1 1 calc R U . . .
C11 C 0.1651(4) 0.2164(3) 0.5188(2) 0.0219(7) Uani 1 1 d . . . . .
H11 H 0.0596 0.2017 0.5202 0.026 Uiso 1 1 calc R U . . .
C17 C 0.1051(4) -0.0366(3) 0.7374(2) 0.0235(7) Uani 1 1 d . . . . .
H17 H 0.0670 -0.0032 0.7836 0.028 Uiso 1 1 calc R U . . .
C28 C 0.1960(4) 0.7025(3) 0.9634(2) 0.0275(8) Uani 1 1 d . . . . .
H28 H 0.1680 0.7560 0.9988 0.033 Uiso 1 1 calc R U . . .
C30 C 0.3104(4) 0.6467(3) 0.8380(2) 0.0234(7) Uani 1 1 d . . . . .
H30 H 0.3597 0.6635 0.7896 0.028 Uiso 1 1 calc R U . . .
C13 C 0.2205(4) -0.0289(3) 0.6045(2) 0.0257(8) Uani 1 1 d . . . . .
H13 H 0.2606 0.0094 0.5613 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4802(4) 0.2604(3) 0.5138(2) 0.0295(8) Uani 1 1 d . . . . .
H8 H 0.5857 0.2756 0.5121 0.035 Uiso 1 1 calc R U . . .
C26 C 0.2017(4) 0.5160(3) 0.9288(2) 0.0209(7) Uani 1 1 d . . . . .
H26 H 0.1790 0.4456 0.9418 0.025 Uiso 1 1 calc R U . . .
C21 C -0.0299(4) 0.3452(3) 0.7147(2) 0.0174(6) Uani 1 1 d . . . . .
H21A H -0.1112 0.3785 0.7220 0.021 Uiso 1 1 calc R U . . .
H21B H 0.0197 0.3493 0.7713 0.021 Uiso 1 1 calc R U . . .
C9 C 0.3886(5) 0.2645(3) 0.4423(2) 0.0314(9) Uani 1 1 d . . . . .
H9 H 0.4329 0.2808 0.3923 0.038 Uiso 1 1 calc R U . . .
C10 C 0.2329(5) 0.2445(3) 0.4452(2) 0.0280(8) Uani 1 1 d . . . . .
H10 H 0.1729 0.2497 0.3978 0.034 Uiso 1 1 calc R U . . .
C20 C -0.2796(4) 0.0869(3) 0.6253(2) 0.0291(8) Uani 1 1 d . . . . .
H20 H -0.3768 0.0388 0.6051 0.035 Uiso 1 1 calc R U . . .
C29 C 0.2716(4) 0.7281(3) 0.8924(2) 0.0278(8) Uani 1 1 d . . . . .
H29 H 0.2967 0.7992 0.8807 0.033 Uiso 1 1 calc R U . . .
C1 C 0.3906(4) 0.2351(3) 0.9434(2) 0.0247(7) Uani 1 1 d . . . . .
H1 H 0.3414 0.2374 0.9934 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4977(4) 0.3245(3) 0.9182(2) 0.0258(8) Uani 1 1 d . . . . .
H2 H 0.5326 0.3958 0.9486 0.031 Uiso 1 1 calc R U . . .
C34 C 0.8533(4) 0.5925(3) 0.7842(3) 0.0283(8) Uani 1 1 d . . . . .
H34 H 0.9598 0.6189 0.7860 0.034 Uiso 1 1 calc R U . . .
C35 C 0.7656(4) 0.5363(3) 0.7078(2) 0.0278(8) Uani 1 1 d . . . . .
H35 H 0.8137 0.5283 0.6579 0.033 Uiso 1 1 calc R U . . .
C3 C 0.5441(4) 0.2863(3) 0.8370(2) 0.0262(8) Uani 1 1 d . . . . .
H3 H 0.6129 0.3286 0.8049 0.031 Uiso 1 1 calc R U . . .
C4 C 0.4654(4) 0.1721(3) 0.8149(2) 0.0262(8) Uani 1 1 d . . . . .
H4 H 0.4756 0.1262 0.7659 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3695(4) 0.1395(3) 0.8793(2) 0.0257(8) Uani 1 1 d . . . . .
H5 H 0.3046 0.0692 0.8802 0.031 Uiso 1 1 calc R U . . .
C15 C 0.1570(5) -0.1957(3) 0.6634(3) 0.0385(10) Uani 1 1 d . . . . .
H15 H 0.1552 -0.2683 0.6606 0.046 Uiso 1 1 calc R U . . .
C14 C 0.2150(5) -0.1389(3) 0.5998(3) 0.0370(9) Uani 1 1 d . . . . .
H14 H 0.2510 -0.1735 0.5533 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C3 2.189(3) . ?
Ru1 C4 2.197(3) . ?
Ru1 C5 2.220(3) . ?
Ru1 C2 2.223(3) . ?
Ru1 C1 2.228(3) . ?
Ru1 P1 2.2919(8) . ?
Ru1 P2 2.3060(8) . ?
Ru1 Cl1 2.4581(8) . ?
P2 C22 1.830(3) . ?
P2 C31 1.842(3) . ?
P2 C25 1.844(3) . ?
P1 C18 1.829(3) . ?
P1 C6 1.830(3) . ?
P1 C12 1.840(3) . ?
N1 N2 1.364(4) . ?
N1 C18 1.370(4) . ?
N1 C21 1.447(4) . ?
N3 N4 1.361(4) . ?
N3 C22 1.372(4) . ?
N3 C21 1.440(4) . ?
N2 C20 1.328(5) . ?
N4 C24 1.327(5) . ?
C33 C34 1.381(5) . ?
C33 C32 1.389(5) . ?
C33 H33 0.9300 . ?
C32 C31 1.393(5) . ?
C32 H32 0.9300 . ?
C22 C23 1.388(5) . ?
C6 C11 1.394(5) . ?
C6 C7 1.396(5) . ?
C18 C19 1.371(5) . ?
C12 C13 1.388(5) . ?
C12 C17 1.400(5) . ?
C23 C24 1.393(5) . ?
C23 H23 0.9300 . ?
C25 C26 1.387(5) . ?
C25 C30 1.398(5) . ?
C7 C8 1.388(5) . ?
C7 H7 0.9300 . ?
C24 H24 0.9300 . ?
C31 C36 1.396(5) . ?
C19 C20 1.396(5) . ?
C19 H19 0.9300 . ?
C36 C35 1.391(5) . ?
C36 H36 0.9300 . ?
C27 C28 1.385(5) . ?
C27 C26 1.395(5) . ?
C27 H27 0.9300 . ?
C16 C17 1.377(5) . ?
C16 C15 1.385(6) . ?
C16 H16 0.9300 . ?
C11 C10 1.393(5) . ?
C11 H11 0.9300 . ?
C17 H17 0.9300 . ?
C28 C29 1.380(5) . ?
C28 H28 0.9300 . ?
C30 C29 1.399(5) . ?
C30 H30 0.9300 . ?
C13 C14 1.402(5) . ?
C13 H13 0.9300 . ?
C8 C9 1.391(6) . ?
C8 H8 0.9300 . ?
C26 H26 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.376(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C20 H20 0.9300 . ?
C29 H29 0.9300 . ?
C1 C2 1.401(5) . ?
C1 C5 1.437(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.436(5) . ?
C2 H2 0.9300 . ?
C34 C35 1.388(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C3 C4 1.421(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.409(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C15 C14 1.371(6) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?

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
C3 Ru1 C4 37.80(14) . . ?
C3 Ru1 C5 62.97(14) . . ?
C4 Ru1 C5 37.19(14) . . ?
C3 Ru1 C2 37.98(13) . . ?
C4 Ru1 C2 62.73(14) . . ?
C5 Ru1 C2 62.51(14) . . ?
C3 Ru1 C1 62.59(13) . . ?
C4 Ru1 C1 62.32(13) . . ?
C5 Ru1 C1 37.69(13) . . ?
C2 Ru1 C1 36.70(13) . . ?
C3 Ru1 P1 115.89(10) . . ?
C4 Ru1 P1 92.45(10) . . ?
C5 Ru1 P1 104.32(10) . . ?
C2 Ru1 P1 153.28(10) . . ?
C1 Ru1 P1 140.93(10) . . ?
C3 Ru1 P2 94.02(10) . . ?
C4 Ru1 P2 127.45(11) . . ?
C5 Ru1 P2 154.54(10) . . ?
C2 Ru1 P2 92.83(10) . . ?
C1 Ru1 P2 123.55(10) . . ?
P1 Ru1 P2 95.33(3) . . ?
C3 Ru1 Cl1 149.85(9) . . ?
C4 Ru1 Cl1 131.63(10) . . ?
C5 Ru1 Cl1 95.96(10) . . ?
C2 Ru1 Cl1 114.34(10) . . ?
C1 Ru1 Cl1 87.45(10) . . ?
P1 Ru1 Cl1 89.12(3) . . ?
P2 Ru1 Cl1 100.43(3) . . ?
C22 P2 C31 102.58(15) . . ?
C22 P2 C25 97.57(14) . . ?
C31 P2 C25 100.25(14) . . ?
C22 P2 Ru1 120.59(11) . . ?
C31 P2 Ru1 111.29(10) . . ?
C25 P2 Ru1 121.23(11) . . ?
C18 P1 C6 102.49(14) . . ?
C18 P1 C12 98.52(15) . . ?
C6 P1 C12 102.25(15) . . ?
C18 P1 Ru1 119.88(10) . . ?
C6 P1 Ru1 118.84(11) . . ?
C12 P1 Ru1 111.71(11) . . ?
N2 N1 C18 112.4(3) . . ?
N2 N1 C21 117.7(3) . . ?
C18 N1 C21 129.7(3) . . ?
N4 N3 C22 112.6(3) . . ?
N4 N3 C21 119.1(3) . . ?
C22 N3 C21 128.2(3) . . ?
C20 N2 N1 103.7(3) . . ?
C24 N4 N3 104.2(3) . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C32 C31 121.6(3) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
N3 C22 C23 105.3(3) . . ?
N3 C22 P2 120.4(2) . . ?
C23 C22 P2 134.1(3) . . ?
C11 C6 C7 119.2(3) . . ?
C11 C6 P1 123.0(3) . . ?
C7 C6 P1 117.8(2) . . ?
N1 C18 C19 105.9(3) . . ?
N1 C18 P1 124.6(2) . . ?
C19 C18 P1 129.5(3) . . ?
C13 C12 C17 119.0(3) . . ?
C13 C12 P1 123.5(3) . . ?
C17 C12 P1 117.4(2) . . ?
C22 C23 C24 105.4(3) . . ?
C22 C23 H23 127.3 . . ?
C24 C23 H23 127.3 . . ?
C26 C25 C30 119.5(3) . . ?
C26 C25 P2 120.8(3) . . ?
C30 C25 P2 119.7(2) . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N4 C24 C23 112.5(3) . . ?
N4 C24 H24 123.7 . . ?
C23 C24 H24 123.7 . . ?
C32 C31 C36 118.4(3) . . ?
C32 C31 P2 118.5(2) . . ?
C36 C31 P2 122.4(2) . . ?
C18 C19 C20 105.5(3) . . ?
C18 C19 H19 127.3 . . ?
C20 C19 H19 127.3 . . ?
C35 C36 C31 119.9(3) . . ?
C35 C36 H36 120.1 . . ?
C31 C36 H36 120.1 . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C17 C16 C15 120.7(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C10 C11 C6 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C6 C11 H11 119.9 . . ?
C16 C17 C12 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C12 C17 H17 119.9 . . ?
C29 C28 C27 120.2(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C25 C30 C29 120.2(3) . . ?
C25 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C25 C26 C27 119.9(3) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
N3 C21 N1 113.0(3) . . ?
N3 C21 H21A 109.0 . . ?
N1 C21 H21A 109.0 . . ?
N3 C21 H21B 109.0 . . ?
N1 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
N2 C20 C19 112.5(3) . . ?
N2 C20 H20 123.8 . . ?
C19 C20 H20 123.8 . . ?
C28 C29 C30 119.8(3) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C2 C1 C5 108.6(3) . . ?
C2 C1 Ru1 71.45(18) . . ?
C5 C1 Ru1 70.84(18) . . ?
C2 C1 H1 125.7 . . ?
C5 C1 H1 125.7 . . ?
Ru1 C1 H1 123.6 . . ?
C1 C2 C3 107.9(3) . . ?
C1 C2 Ru1 71.85(19) . . ?
C3 C2 Ru1 69.73(18) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
Ru1 C2 H2 124.0 . . ?
C33 C34 C35 119.5(3) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 121.0(3) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C4 C3 C2 107.3(3) . . ?
C4 C3 Ru1 71.41(19) . . ?
C2 C3 Ru1 72.28(19) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
Ru1 C3 H3 121.7 . . ?
C5 C4 C3 108.9(3) . . ?
C5 C4 Ru1 72.26(19) . . ?
C3 C4 Ru1 70.79(19) . . ?
C5 C4 H4 125.5 . . ?
C3 C4 H4 125.5 . . ?
Ru1 C4 H4 123.0 . . ?
C4 C5 C1 107.2(3) . . ?
C4 C5 Ru1 70.54(19) . . ?
C1 C5 Ru1 71.47(18) . . ?
C4 C5 H5 126.4 . . ?
C1 C5 H5 126.4 . . ?
Ru1 C5 H5 123.3 . . ?
C14 C15 C16 119.7(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 N1 N2 C20 -0.1(4) . . . . ?
C21 N1 N2 C20 -175.3(3) . . . . ?
C22 N3 N4 C24 0.1(4) . . . . ?
C21 N3 N4 C24 177.2(3) . . . . ?
C34 C33 C32 C31 1.3(5) . . . . ?
N4 N3 C22 C23 0.2(4) . . . . ?
C21 N3 C22 C23 -176.7(3) . . . . ?
N4 N3 C22 P2 175.7(2) . . . . ?
C21 N3 C22 P2 -1.2(4) . . . . ?
C31 P2 C22 N3 -179.1(2) . . . . ?
C25 P2 C22 N3 -76.8(3) . . . . ?
Ru1 P2 C22 N3 56.6(3) . . . . ?
C31 P2 C22 C23 -5.1(4) . . . . ?
C25 P2 C22 C23 97.2(3) . . . . ?
Ru1 P2 C22 C23 -129.5(3) . . . . ?
C18 P1 C6 C11 -2.8(3) . . . . ?
C12 P1 C6 C11 98.9(3) . . . . ?
Ru1 P1 C6 C11 -137.6(2) . . . . ?
C18 P1 C6 C7 179.2(3) . . . . ?
C12 P1 C6 C7 -79.1(3) . . . . ?
Ru1 P1 C6 C7 44.4(3) . . . . ?
N2 N1 C18 C19 0.2(4) . . . . ?
C21 N1 C18 C19 174.7(3) . . . . ?
N2 N1 C18 P1 -179.9(2) . . . . ?
C21 N1 C18 P1 -5.3(5) . . . . ?
C6 P1 C18 N1 -84.8(3) . . . . ?
C12 P1 C18 N1 170.6(3) . . . . ?
Ru1 P1 C18 N1 49.4(3) . . . . ?
C6 P1 C18 C19 95.2(3) . . . . ?
C12 P1 C18 C19 -9.5(3) . . . . ?
Ru1 P1 C18 C19 -130.6(3) . . . . ?
C18 P1 C12 C13 108.0(3) . . . . ?
C6 P1 C12 C13 3.1(3) . . . . ?
Ru1 P1 C12 C13 -125.0(3) . . . . ?
C18 P1 C12 C17 -73.7(3) . . . . ?
C6 P1 C12 C17 -178.6(3) . . . . ?
Ru1 P1 C12 C17 53.3(3) . . . . ?
N3 C22 C23 C24 -0.3(4) . . . . ?
P2 C22 C23 C24 -174.9(3) . . . . ?
C22 P2 C25 C26 127.1(3) . . . . ?
C31 P2 C25 C26 -128.6(3) . . . . ?
Ru1 P2 C25 C26 -5.8(3) . . . . ?
C22 P2 C25 C30 -53.5(3) . . . . ?
C31 P2 C25 C30 50.8(3) . . . . ?
Ru1 P2 C25 C30 173.5(2) . . . . ?
C11 C6 C7 C8 -1.4(5) . . . . ?
P1 C6 C7 C8 176.7(3) . . . . ?
N3 N4 C24 C23 -0.3(4) . . . . ?
C22 C23 C24 N4 0.4(4) . . . . ?
C33 C32 C31 C36 -1.6(5) . . . . ?
C33 C32 C31 P2 168.9(3) . . . . ?
C22 P2 C31 C32 143.4(3) . . . . ?
C25 P2 C31 C32 43.2(3) . . . . ?
Ru1 P2 C31 C32 -86.3(3) . . . . ?
C22 P2 C31 C36 -46.5(3) . . . . ?
C25 P2 C31 C36 -146.8(3) . . . . ?
Ru1 P2 C31 C36 83.7(3) . . . . ?
N1 C18 C19 C20 -0.2(4) . . . . ?
P1 C18 C19 C20 179.8(3) . . . . ?
C32 C31 C36 C35 -0.5(5) . . . . ?
P2 C31 C36 C35 -170.5(3) . . . . ?
C7 C6 C11 C10 0.7(5) . . . . ?
P1 C6 C11 C10 -177.3(3) . . . . ?
C15 C16 C17 C12 -0.1(6) . . . . ?
C13 C12 C17 C16 0.8(5) . . . . ?
P1 C12 C17 C16 -177.6(3) . . . . ?
C26 C27 C28 C29 -0.8(5) . . . . ?
C26 C25 C30 C29 0.0(5) . . . . ?
P2 C25 C30 C29 -179.3(3) . . . . ?
C17 C12 C13 C14 -0.6(5) . . . . ?
P1 C12 C13 C14 177.7(3) . . . . ?
C6 C7 C8 C9 0.3(5) . . . . ?
C30 C25 C26 C27 0.8(5) . . . . ?
P2 C25 C26 C27 -179.9(2) . . . . ?
C28 C27 C26 C25 -0.4(5) . . . . ?
N4 N3 C21 N1 72.6(3) . . . . ?
C22 N3 C21 N1 -110.7(3) . . . . ?
N2 N1 C21 N3 -117.6(3) . . . . ?
C18 N1 C21 N3 68.1(4) . . . . ?
C7 C8 C9 C10 1.5(6) . . . . ?
C8 C9 C10 C11 -2.2(5) . . . . ?
C6 C11 C10 C9 1.1(5) . . . . ?
N1 N2 C20 C19 -0.1(4) . . . . ?
C18 C19 C20 N2 0.2(4) . . . . ?
C27 C28 C29 C30 1.6(5) . . . . ?
C25 C30 C29 C28 -1.2(5) . . . . ?
C5 C1 C2 C3 0.7(4) . . . . ?
Ru1 C1 C2 C3 -60.7(2) . . . . ?
C5 C1 C2 Ru1 61.4(2) . . . . ?
C32 C33 C34 C35 1.1(5) . . . . ?
C33 C34 C35 C36 -3.1(5) . . . . ?
C31 C36 C35 C34 2.8(5) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
Ru1 C2 C3 C4 -63.3(2) . . . . ?
C1 C2 C3 Ru1 62.1(2) . . . . ?
C2 C3 C4 C5 1.3(4) . . . . ?
Ru1 C3 C4 C5 -62.6(2) . . . . ?
C2 C3 C4 Ru1 63.8(2) . . . . ?
C3 C4 C5 C1 -0.8(4) . . . . ?
Ru1 C4 C5 C1 -62.5(2) . . . . ?
C3 C4 C5 Ru1 61.6(2) . . . . ?
C2 C1 C5 C4 0.1(4) . . . . ?
Ru1 C1 C5 C4 61.9(2) . . . . ?
C2 C1 C5 Ru1 -61.8(2) . . . . ?
C17 C16 C15 C14 -0.8(6) . . . . ?
C16 C15 C14 C13 1.1(6) . . . . ?
C12 C13 C14 C15 -0.4(6) . . . . ?

_refine_diff_density_max         0.580
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.109



####################################################################### 
# 
# 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_Compound-12
_database_code_depnum_ccdc_archive 'CCDC 1517754'
_audit_update_record             
;
2016-11-17 deposited with the CCDC.
2016-11-23 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         'C35 H31 Cl3 N6 P2 Ru'
_chemical_formula_sum            'C35 H31 Cl3 N6 P2 Ru'
_chemical_formula_weight         805.02

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'
N N 0.0061 0.0033 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4977(3)
_cell_length_b                   18.3954(4)
_cell_length_c                   19.9460(5)
_cell_angle_alpha                87.8663(17)
_cell_angle_beta                 79.437(2)
_cell_angle_gamma                78.663(2)
_cell_volume                     3358.93(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    37015
_cell_measurement_theta_min      2.2230
_cell_measurement_theta_max      31.2400

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_F_000             1632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.838
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.90277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'NUMABS RIGAKU 1999'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku saturn 724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            57268
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.223
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11835
_reflns_number_gt                10644
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0270P)²+3.5500P] 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         11835
_refine_ls_number_parameters     847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.98756(2) -0.02128(2) 0.30855(2) 0.01283(5) Uani 1 1 d . . . . .
Ru1A Ru 0.47975(2) 0.51214(2) 0.22816(2) 0.01609(6) Uani 1 1 d . . . . .
Cl1 Cl 0.77503(7) -0.08066(3) 0.32888(3) 0.02174(13) Uani 1 1 d . . . . .
P2 P 0.89187(7) 0.08939(3) 0.36374(3) 0.01403(13) Uani 1 1 d . . . . .
Cl1A Cl 0.42303(7) 0.43515(3) 0.32761(3) 0.02373(14) Uani 1 1 d . . . . .
P1 P 0.92776(6) 0.01643(3) 0.20550(3) 0.01351(13) Uani 1 1 d . . . . .
P1A P 0.34522(7) 0.61924(3) 0.28029(3) 0.01629(13) Uani 1 1 d . . . . .
P2A P 0.29927(7) 0.47467(3) 0.18450(3) 0.01629(13) Uani 1 1 d . . . . .
Cl2 Cl 1.20848(8) 0.22563(4) -0.04855(4) 0.03660(17) Uani 1 1 d . . . . .
Cl3 Cl 1.38527(9) 0.09048(4) -0.00417(4) 0.03881(18) Uani 1 1 d . . . . .
Cl3A Cl 0.19110(9) 0.47716(4) 0.50071(4) 0.0454(2) Uani 1 1 d . . . . .
Cl2A Cl 0.20786(10) 0.32619(5) 0.55117(4) 0.0494(2) Uani 1 1 d . . . . .
N2A N -0.0757(2) 0.62851(12) 0.27740(11) 0.0236(5) Uani 1 1 d . . . . .
N3 N 0.6157(2) 0.06006(10) 0.23513(10) 0.0163(4) Uani 1 1 d . . . . .
N2 N 0.4948(2) 0.06093(11) 0.20707(11) 0.0215(5) Uani 1 1 d . . . . .
N1A N 0.0882(2) 0.70142(11) 0.23817(11) 0.0230(5) Uani 1 1 d . . . . .
N3A N 0.0571(2) 0.59942(11) 0.29347(10) 0.0174(4) Uani 1 1 d . . . . .
N5A N -0.0180(2) 0.42221(11) 0.32991(11) 0.0219(5) Uani 1 1 d . . . . .
N4A N 0.0728(2) 0.46762(11) 0.29965(10) 0.0179(4) Uani 1 1 d . . . . .
N1 N 0.6998(2) 0.00579(11) 0.13644(10) 0.0202(4) Uani 1 1 d . . . . .
N4 N 0.6593(2) 0.15647(10) 0.30190(10) 0.0168(4) Uani 1 1 d . . . . .
N6A N 0.1177(2) 0.37285(11) 0.23077(11) 0.0225(5) Uani 1 1 d . . . . .
N5 N 0.5880(2) 0.22241(11) 0.28036(11) 0.0230(5) Uani 1 1 d . . . . .
N6 N 0.7952(2) 0.23593(11) 0.31514(11) 0.0215(5) Uani 1 1 d . . . . .
C19A C -0.0501(3) 0.68870(14) 0.24405(14) 0.0262(6) Uani 1 1 d . . . . .
H19A H -0.1219 0.7207 0.2256 0.031 Uiso 1 1 calc R U . . .
C23 C 0.7590(3) 0.09373(14) 0.44365(12) 0.0185(5) Uani 1 1 d . . . . .
C29 C 1.0293(3) 0.13666(12) 0.38695(12) 0.0172(5) Uani 1 1 d . . . . .
C34 C 1.1091(3) 0.17683(13) 0.33868(13) 0.0208(5) Uani 1 1 d . . . . .
H34 H 1.0859 0.1841 0.2953 0.025 Uiso 1 1 calc R U . . .
C6A C 0.4126(3) 0.70326(13) 0.24927(13) 0.0188(5) Uani 1 1 d . . . . .
C7 C 1.0107(3) -0.12504(13) 0.15020(13) 0.0202(5) Uani 1 1 d . . . . .
H7 H 0.9597 -0.1393 0.1913 0.024 Uiso 1 1 calc R U . . .
C6 C 1.0153(3) -0.05054(13) 0.13745(12) 0.0164(5) Uani 1 1 d . . . . .
C28 C 0.7175(3) 0.03019(15) 0.47306(13) 0.0249(6) Uani 1 1 d . . . . .
H28 H 0.7593 -0.0159 0.4534 0.030 Uiso 1 1 calc R U . . .
C9 C 1.1578(3) -0.15715(15) 0.04046(13) 0.0272(6) Uani 1 1 d . . . . .
H9 H 1.2061 -0.1930 0.0081 0.033 Uiso 1 1 calc R U . . .
C10 C 1.1622(3) -0.08346(15) 0.02704(14) 0.0306(6) Uani 1 1 d . . . . .
H10 H 1.2122 -0.0695 -0.0145 0.037 Uiso 1 1 calc R U . . .
C13 C 1.1089(3) 0.11881(14) 0.17611(13) 0.0232(6) Uani 1 1 d . . . . .
H13 H 1.1761 0.0826 0.1933 0.028 Uiso 1 1 calc R U . . .
C22 C 0.7826(3) 0.16542(13) 0.32252(12) 0.0166(5) Uani 1 1 d . . . . .
C18A C 0.1534(3) 0.64400(12) 0.27021(12) 0.0166(5) Uani 1 1 d . . . . .
C21A C 0.0139(3) 0.36631(13) 0.28633(14) 0.0236(6) Uani 1 1 d . . . . .
H21A H -0.0314 0.3255 0.2932 0.028 Uiso 1 1 calc R U . . .
C18 C 0.7369(3) 0.02711(12) 0.19241(12) 0.0153(5) Uani 1 1 d . . . . .
C12A C 0.3231(3) 0.62838(13) 0.37310(13) 0.0194(5) Uani 1 1 d . . . . .
C13A C 0.1994(3) 0.67180(14) 0.41119(14) 0.0244(6) Uani 1 1 d . . . . .
H13A H 0.1256 0.6970 0.3894 0.029 Uiso 1 1 calc R U . . .
C30A C 0.2683(3) 0.58541(14) 0.08739(14) 0.0259(6) Uani 1 1 d . . . . .
H30A H 0.3586 0.5925 0.0947 0.031 Uiso 1 1 calc R U . . .
C33 C 1.2223(3) 0.20600(14) 0.35479(14) 0.0254(6) Uani 1 1 d . . . . .
H33 H 1.2743 0.2330 0.3224 0.030 Uiso 1 1 calc R U . . .
C23A C 0.3723(3) 0.39208(13) 0.13056(13) 0.0199(5) Uani 1 1 d . . . . .
C25A C 0.4894(3) 0.26347(14) 0.12301(16) 0.0288(6) Uani 1 1 d . . . . .
H25A H 0.5296 0.2203 0.1438 0.035 Uiso 1 1 calc R U . . .
C30 C 1.0658(3) 0.12705(14) 0.45132(13) 0.0232(6) Uani 1 1 d . . . . .
H30 H 1.0129 0.1009 0.4842 0.028 Uiso 1 1 calc R U . . .
C24A C 0.4350(3) 0.32765(14) 0.16115(14) 0.0246(6) Uani 1 1 d . . . . .
H24A H 0.4404 0.3276 0.2072 0.030 Uiso 1 1 calc R U . . .
C9A C 0.5372(3) 0.82371(15) 0.19846(16) 0.0331(7) Uani 1 1 d . . . . .
H9A H 0.5781 0.8641 0.1815 0.040 Uiso 1 1 calc R U . . .
C16 C 0.9118(3) 0.22739(14) 0.12497(13) 0.0288(6) Uani 1 1 d . . . . .
H16 H 0.8454 0.2639 0.1076 0.035 Uiso 1 1 calc R U . . .
C28A C 0.3686(3) 0.39170(15) 0.06140(14) 0.0261(6) Uani 1 1 d . . . . .
H28A H 0.3283 0.4347 0.0403 0.031 Uiso 1 1 calc R U . . .
C14 C 1.1457(3) 0.18643(16) 0.15520(14) 0.0312(7) Uani 1 1 d . . . . .
H14 H 1.2380 0.1949 0.1576 0.037 Uiso 1 1 calc R U . . .
C11 C 1.0916(3) -0.03031(14) 0.07576(13) 0.0254(6) Uani 1 1 d . . . . .
H11 H 1.0954 0.0193 0.0670 0.031 Uiso 1 1 calc R U . . .
C29A C 0.1972(3) 0.53566(13) 0.12828(13) 0.0194(5) Uani 1 1 d . . . . .
C17 C 0.8742(3) 0.15935(13) 0.14478(13) 0.0219(5) Uani 1 1 d . . . . .
H17 H 0.7835 0.1504 0.1400 0.026 Uiso 1 1 calc R U . . .
C20 C 0.5972(3) 0.09074(13) 0.30281(12) 0.0168(5) Uani 1 1 d . . . . .
H20A H 0.4940 0.1029 0.3220 0.020 Uiso 1 1 calc R U . . .
H20B H 0.6436 0.0537 0.3319 0.020 Uiso 1 1 calc R U . . .
C8 C 1.0823(3) -0.17796(14) 0.10154(13) 0.0237(6) Uani 1 1 d . . . . .
H8 H 1.0793 -0.2277 0.1101 0.028 Uiso 1 1 calc R U . . .
C10A C 0.5590(3) 0.79407(15) 0.26092(16) 0.0331(7) Uani 1 1 d . . . . .
H10A H 0.6157 0.8141 0.2859 0.040 Uiso 1 1 calc R U . . .
C31A C 0.2061(3) 0.62435(15) 0.03604(15) 0.0311(6) Uani 1 1 d . . . . .
H31A H 0.2555 0.6565 0.0084 0.037 Uiso 1 1 calc R U . . .
C19 C 0.5521(3) 0.02750(14) 0.14844(13) 0.0228(6) Uani 1 1 d . . . . .
H19 H 0.4952 0.0193 0.1172 0.027 Uiso 1 1 calc R U . . .
C16A C 0.4210(3) 0.60022(15) 0.47665(15) 0.0328(7) Uani 1 1 d . . . . .
H16A H 0.4961 0.5770 0.4986 0.039 Uiso 1 1 calc R U . . .
C11A C 0.4965(3) 0.73427(14) 0.28680(14) 0.0258(6) Uani 1 1 d . . . . .
H11A H 0.5106 0.7148 0.3293 0.031 Uiso 1 1 calc R U . . .
C24 C 0.6952(3) 0.16242(16) 0.47380(14) 0.0309(6) Uani 1 1 d . . . . .
H24 H 0.7228 0.2053 0.4543 0.037 Uiso 1 1 calc R U . . .
C14A C 0.1854(3) 0.67769(15) 0.48127(14) 0.0313(7) Uani 1 1 d . . . . .
H14A H 0.1013 0.7055 0.5065 0.038 Uiso 1 1 calc R U . . .
C27 C 0.6125(3) 0.0356(2) 0.53240(14) 0.0373(8) Uani 1 1 d . . . . .
H27 H 0.5846 -0.0070 0.5524 0.045 Uiso 1 1 calc R U . . .
C15 C 1.0463(3) 0.24116(15) 0.13092(13) 0.0312(7) Uani 1 1 d . . . . .
H15 H 1.0699 0.2871 0.1186 0.037 Uiso 1 1 calc R U . . .
C26A C 0.4843(3) 0.26334(15) 0.05428(16) 0.0329(7) Uani 1 1 d . . . . .
H26A H 0.5208 0.2202 0.0288 0.039 Uiso 1 1 calc R U . . .
C7A C 0.3931(3) 0.73330(14) 0.18564(14) 0.0233(6) Uani 1 1 d . . . . .
H7A H 0.3386 0.7129 0.1597 0.028 Uiso 1 1 calc R U . . .
C12 C 0.9717(3) 0.10467(13) 0.17163(12) 0.0171(5) Uani 1 1 d . . . . .
C31 C 1.1800(3) 0.15584(15) 0.46735(14) 0.0286(6) Uani 1 1 d . . . . .
H31 H 1.2037 0.1487 0.5106 0.034 Uiso 1 1 calc R U . . .
C21 C 0.6744(3) 0.26744(14) 0.28931(14) 0.0251(6) Uani 1 1 d . . . . .
H21 H 0.6543 0.3176 0.2787 0.030 Uiso 1 1 calc R U . . .
C8A C 0.4546(3) 0.79340(14) 0.16089(15) 0.0297(6) Uani 1 1 d . . . . .
H8A H 0.4402 0.8135 0.1186 0.036 Uiso 1 1 calc R U . . .
C32 C 1.2582(3) 0.19513(14) 0.41877(15) 0.0282(6) Uani 1 1 d . . . . .
H32 H 1.3352 0.2143 0.4293 0.034 Uiso 1 1 calc R U . . .
C17A C 0.4345(3) 0.59244(14) 0.40645(14) 0.0266(6) Uani 1 1 d . . . . .
H17A H 0.5178 0.5633 0.3818 0.032 Uiso 1 1 calc R U . . .
C1 C 1.1062(3) -0.11600(13) 0.36064(13) 0.0228(6) Uani 1 1 d . . . . .
H1 H 1.0599 -0.1475 0.3906 0.027 Uiso 1 1 calc R U . . .
C20A C 0.0769(3) 0.53386(13) 0.33585(13) 0.0192(5) Uani 1 1 d . . . . .
H20C H 0.0006 0.5400 0.3760 0.023 Uiso 1 1 calc R U . . .
H20D H 0.1699 0.5282 0.3509 0.023 Uiso 1 1 calc R U . . .
C15A C 0.2970(4) 0.64201(16) 0.51364(15) 0.0345(7) Uani 1 1 d . . . . .
H15A H 0.2881 0.6463 0.5606 0.041 Uiso 1 1 calc R U . . .
C5 C 1.1494(3) -0.12633(13) 0.28890(13) 0.0217(5) Uani 1 1 d . . . . .
H5 H 1.1363 -0.1652 0.2637 0.026 Uiso 1 1 calc R U . . .
C22A C 0.1543(3) 0.43708(13) 0.24126(12) 0.0174(5) Uani 1 1 d . . . . .
C32A C 0.0707(3) 0.61548(16) 0.02578(15) 0.0334(7) Uani 1 1 d . . . . .
H32A H 0.0290 0.6415 -0.0089 0.040 Uiso 1 1 calc R U . . .
C34A C 0.0603(3) 0.52761(16) 0.11788(14) 0.0297(6) Uani 1 1 d . . . . .
H34A H 0.0109 0.4951 0.1451 0.036 Uiso 1 1 calc R U . . .
C2 C 1.1450(3) -0.05059(14) 0.37872(13) 0.0227(6) Uani 1 1 d . . . . .
H2 H 1.1299 -0.0316 0.4226 0.027 Uiso 1 1 calc R U . . .
C27A C 0.4248(3) 0.32746(16) 0.02378(15) 0.0345(7) Uani 1 1 d . . . . .
H27A H 0.4222 0.3277 -0.0226 0.041 Uiso 1 1 calc R U . . .
C4 C 1.2158(3) -0.06635(14) 0.26328(13) 0.0221(5) Uani 1 1 d . . . . .
H4 H 1.2558 -0.0594 0.2179 0.027 Uiso 1 1 calc R U . . .
C35 C 1.2122(3) 0.13308(15) -0.02196(15) 0.0308(6) Uani 1 1 d . . . . .
H35A H 1.1885 0.1054 -0.0574 0.037 Uiso 1 1 calc R U . . .
H35B H 1.1388 0.1318 0.0186 0.037 Uiso 1 1 calc R U . . .
C25 C 0.5911(3) 0.1668(2) 0.53255(15) 0.0417(8) Uani 1 1 d . . . . .
H25 H 0.5488 0.2127 0.5525 0.050 Uiso 1 1 calc R U . . .
C26 C 0.5499(3) 0.1036(2) 0.56170(15) 0.0447(9) Uani 1 1 d . . . . .
H26 H 0.4797 0.1068 0.6012 0.054 Uiso 1 1 calc R U . . .
C3A C 0.6801(3) 0.44041(15) 0.17324(15) 0.0291(6) Uani 1 1 d . . . . .
H3A H 0.6895 0.3897 0.1669 0.035 Uiso 1 1 calc R U . . .
C33A C -0.0029(3) 0.56784(18) 0.06714(15) 0.0379(7) Uani 1 1 d . . . . .
H33A H -0.0951 0.5627 0.0609 0.045 Uiso 1 1 calc R U . . .
C1A C 0.6301(3) 0.56688(15) 0.15765(15) 0.0275(6) Uani 1 1 d . . . . .
H1A H 0.5995 0.6134 0.1395 0.033 Uiso 1 1 calc R U . . .
C2A C 0.6270(3) 0.49765(15) 0.12974(14) 0.0285(6) Uani 1 1 d . . . . .
H2A H 0.5953 0.4909 0.0894 0.034 Uiso 1 1 calc R U . . .
C3 C 1.2117(3) -0.01838(14) 0.31775(14) 0.0224(6) Uani 1 1 d . . . . .
H3 H 1.2460 0.0258 0.3145 0.027 Uiso 1 1 calc R U . . .
C4A C 0.7161(3) 0.47514(17) 0.22848(16) 0.0344(7) Uani 1 1 d . . . . .
H4A H 0.7522 0.4507 0.2653 0.041 Uiso 1 1 calc R U . . .
C5A C 0.6887(3) 0.55214(16) 0.21873(15) 0.0306(7) Uani 1 1 d . . . . .
H5A H 0.7056 0.5873 0.2470 0.037 Uiso 1 1 calc R U . . .
C35A C 0.1901(5) 0.38544(19) 0.48012(18) 0.0543(10) Uani 1 1 d . . . . .
H35C H 0.2699 0.3686 0.4429 0.065 Uiso 1 1 calc R U . . .
H35D H 0.0995 0.3834 0.4650 0.065 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C3 2.181(2) . ?
Ru1 C4 2.198(2) . ?
Ru1 C2 2.209(2) . ?
Ru1 C1 2.215(2) . ?
Ru1 C5 2.218(2) . ?
Ru1 P1 2.2794(6) . ?
Ru1 P2 2.2924(6) . ?
Ru1 Cl1 2.4426(6) . ?
Ru1A C1A 2.180(3) . ?
Ru1A C2A 2.183(3) . ?
Ru1A C4A 2.216(3) . ?
Ru1A C3A 2.218(3) . ?
Ru1A C5A 2.223(3) . ?
Ru1A P2A 2.2864(6) . ?
Ru1A P1A 2.2959(6) . ?
Ru1A Cl1A 2.4352(6) . ?
P2 C22 1.835(2) . ?
P2 C23 1.836(2) . ?
P2 C29 1.836(2) . ?
P1 C12 1.829(2) . ?
P1 C6 1.833(2) . ?
P1 C18 1.850(2) . ?
P1A C6A 1.831(2) . ?
P1A C12A 1.835(3) . ?
P1A C18A 1.835(2) . ?
P2A C29A 1.826(3) . ?
P2A C23A 1.839(2) . ?
P2A C22A 1.844(2) . ?
Cl2 C35 1.760(3) . ?
Cl3 C35 1.768(3) . ?
Cl3A C35A 1.754(3) . ?
Cl2A C35A 1.768(4) . ?
N2A C19A 1.311(3) . ?
N2A N3A 1.360(3) . ?
N3 C18 1.350(3) . ?
N3 N2 1.364(3) . ?
N3 C20 1.450(3) . ?
N2 C19 1.315(3) . ?
N1A C18A 1.321(3) . ?
N1A C19A 1.362(3) . ?
N3A C18A 1.355(3) . ?
N3A C20A 1.448(3) . ?
N5A C21A 1.324(3) . ?
N5A N4A 1.364(3) . ?
N4A C22A 1.349(3) . ?
N4A C20A 1.450(3) . ?
N1 C18 1.325(3) . ?
N1 C19 1.360(3) . ?
N4 C22 1.351(3) . ?
N4 N5 1.363(3) . ?
N4 C20 1.444(3) . ?
N6A C22A 1.329(3) . ?
N6A C21A 1.361(3) . ?
N5 C21 1.312(3) . ?
N6 C22 1.326(3) . ?
N6 C21 1.361(3) . ?
C19A H19A 0.9300 . ?
C23 C28 1.382(4) . ?
C23 C24 1.396(4) . ?
C29 C30 1.386(4) . ?
C29 C34 1.395(3) . ?
C34 C33 1.384(4) . ?
C34 H34 0.9300 . ?
C6A C7A 1.394(4) . ?
C6A C11A 1.396(4) . ?
C7 C8 1.386(3) . ?
C7 C6 1.392(3) . ?
C7 H7 0.9300 . ?
C6 C11 1.386(3) . ?
C28 C27 1.393(4) . ?
C28 H28 0.9300 . ?
C9 C8 1.378(4) . ?
C9 C10 1.379(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9300 . ?
C13 C14 1.387(4) . ?
C13 C12 1.397(3) . ?
C13 H13 0.9300 . ?
C21A H21A 0.9300 . ?
C12A C13A 1.394(4) . ?
C12A C17A 1.396(4) . ?
C13A C14A 1.386(4) . ?
C13A H13A 0.9300 . ?
C30A C31A 1.383(4) . ?
C30A C29A 1.394(4) . ?
C30A H30A 0.9300 . ?
C33 C32 1.378(4) . ?
C33 H33 0.9300 . ?
C23A C28A 1.387(4) . ?
C23A C24A 1.390(4) . ?
C25A C26A 1.381(4) . ?
C25A C24A 1.387(4) . ?
C25A H25A 0.9300 . ?
C30 C31 1.387(4) . ?
C30 H30 0.9300 . ?
C24A H24A 0.9300 . ?
C9A C10A 1.375(4) . ?
C9A C8A 1.381(4) . ?
C9A H9A 0.9300 . ?
C16 C15 1.377(4) . ?
C16 C17 1.392(4) . ?
C16 H16 0.9300 . ?
C28A C27A 1.384(4) . ?
C28A H28A 0.9300 . ?
C14 C15 1.377(4) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C29A C34A 1.390(4) . ?
C17 C12 1.390(4) . ?
C17 H17 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C8 H8 0.9300 . ?
C10A C11A 1.390(4) . ?
C10A H10A 0.9300 . ?
C31A C32A 1.380(4) . ?
C31A H31A 0.9300 . ?
C19 H19 0.9300 . ?
C16A C15A 1.374(4) . ?
C16A C17A 1.392(4) . ?
C16A H16A 0.9300 . ?
C11A H11A 0.9300 . ?
C24 C25 1.381(4) . ?
C24 H24 0.9300 . ?
C14A C15A 1.385(4) . ?
C14A H14A 0.9300 . ?
C27 C26 1.376(5) . ?
C27 H27 0.9300 . ?
C15 H15 0.9300 . ?
C26A C27A 1.375(4) . ?
C26A H26A 0.9300 . ?
C7A C8A 1.384(4) . ?
C7A H7A 0.9300 . ?
C31 C32 1.381(4) . ?
C31 H31 0.9300 . ?
C21 H21 0.9300 . ?
C8A H8A 0.9300 . ?
C32 H32 0.9300 . ?
C17A H17A 0.9300 . ?
C1 C2 1.403(4) . ?
C1 C5 1.423(4) . ?
C1 H1 0.9300 . ?
C20A H20C 0.9700 . ?
C20A H20D 0.9700 . ?
C15A H15A 0.9300 . ?
C5 C4 1.411(4) . ?
C5 H5 0.9300 . ?
C32A C33A 1.383(4) . ?
C32A H32A 0.9300 . ?
C34A C33A 1.387(4) . ?
C34A H34A 0.9300 . ?
C2 C3 1.429(4) . ?
C2 H2 0.9300 . ?
C27A H27A 0.9300 . ?
C4 C3 1.415(4) . ?
C4 H4 0.9300 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C25 C26 1.374(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C3A C2A 1.414(4) . ?
C3A C4A 1.420(4) . ?
C3A H3A 0.9300 . ?
C33A H33A 0.9300 . ?
C1A C2A 1.416(4) . ?
C1A C5A 1.425(4) . ?
C1A H1A 0.9300 . ?
C2A H2A 0.9300 . ?
C3 H3 0.9300 . ?
C4A C5A 1.402(4) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
C35A H35C 0.9700 . ?
C35A H35D 0.9700 . ?

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
C3 Ru1 C4 37.71(9) . . ?
C3 Ru1 C2 38.00(10) . . ?
C4 Ru1 C2 62.61(10) . . ?
C3 Ru1 C1 62.75(10) . . ?
C4 Ru1 C1 62.15(10) . . ?
C2 Ru1 C1 36.98(9) . . ?
C3 Ru1 C5 63.10(9) . . ?
C4 Ru1 C5 37.26(9) . . ?
C2 Ru1 C5 62.60(9) . . ?
C1 Ru1 C5 37.46(9) . . ?
C3 Ru1 P1 114.80(7) . . ?
C4 Ru1 P1 92.80(7) . . ?
C2 Ru1 P1 152.54(7) . . ?
C1 Ru1 P1 142.55(7) . . ?
C5 Ru1 P1 105.88(7) . . ?
C3 Ru1 P2 94.21(7) . . ?
C4 Ru1 P2 128.70(7) . . ?
C2 Ru1 P2 90.78(7) . . ?
C1 Ru1 P2 120.84(7) . . ?
C5 Ru1 P2 153.15(7) . . ?
P1 Ru1 P2 96.43(2) . . ?
C3 Ru1 Cl1 151.36(7) . . ?
C4 Ru1 Cl1 130.02(7) . . ?
C2 Ru1 Cl1 116.89(7) . . ?
C1 Ru1 Cl1 88.62(7) . . ?
C5 Ru1 Cl1 94.95(7) . . ?
P1 Ru1 Cl1 87.79(2) . . ?
P2 Ru1 Cl1 100.75(2) . . ?
C1A Ru1A C2A 37.87(10) . . ?
C1A Ru1A C4A 62.59(11) . . ?
C2A Ru1A C4A 62.30(11) . . ?
C1A Ru1A C3A 63.13(10) . . ?
C2A Ru1A C3A 37.47(11) . . ?
C4A Ru1A C3A 37.36(11) . . ?
C1A Ru1A C5A 37.76(11) . . ?
C2A Ru1A C5A 62.60(10) . . ?
C4A Ru1A C5A 36.82(10) . . ?
C3A Ru1A C5A 62.36(10) . . ?
C1A Ru1A P2A 116.60(8) . . ?
C2A Ru1A P2A 91.75(7) . . ?
C4A Ru1A P2A 138.58(8) . . ?
C3A Ru1A P2A 102.53(8) . . ?
C5A Ru1A P2A 153.24(8) . . ?
C1A Ru1A P1A 95.33(7) . . ?
C2A Ru1A P1A 129.27(8) . . ?
C4A Ru1A P1A 122.89(8) . . ?
C3A Ru1A P1A 154.98(7) . . ?
C5A Ru1A P1A 92.93(7) . . ?
P2A Ru1A P1A 98.51(2) . . ?
C1A Ru1A Cl1A 151.87(8) . . ?
C2A Ru1A Cl1A 136.32(8) . . ?
C4A Ru1A Cl1A 90.22(8) . . ?
C3A Ru1A Cl1A 100.22(8) . . ?
C5A Ru1A Cl1A 115.26(8) . . ?
P2A Ru1A Cl1A 88.15(2) . . ?
P1A Ru1A Cl1A 93.78(2) . . ?
C22 P2 C23 94.85(11) . . ?
C22 P2 C29 100.69(11) . . ?
C23 P2 C29 102.11(11) . . ?
C22 P2 Ru1 120.63(8) . . ?
C23 P2 Ru1 120.70(8) . . ?
C29 P2 Ru1 114.08(8) . . ?
C12 P1 C6 104.32(11) . . ?
C12 P1 C18 100.88(11) . . ?
C6 P1 C18 98.67(10) . . ?
C12 P1 Ru1 117.49(8) . . ?
C6 P1 Ru1 112.53(8) . . ?
C18 P1 Ru1 120.21(8) . . ?
C6A P1A C12A 102.36(11) . . ?
C6A P1A C18A 101.55(11) . . ?
C12A P1A C18A 99.78(11) . . ?
C6A P1A Ru1A 114.22(8) . . ?
C12A P1A Ru1A 119.43(8) . . ?
C18A P1A Ru1A 116.79(7) . . ?
C29A P2A C23A 101.35(11) . . ?
C29A P2A C22A 102.43(11) . . ?
C23A P2A C22A 97.22(11) . . ?
C29A P2A Ru1A 120.48(8) . . ?
C23A P2A Ru1A 111.16(8) . . ?
C22A P2A Ru1A 120.31(8) . . ?
C19A N2A N3A 101.8(2) . . ?
C18 N3 N2 110.38(19) . . ?
C18 N3 C20 130.9(2) . . ?
N2 N3 C20 118.72(19) . . ?
C19 N2 N3 101.7(2) . . ?
C18A N1A C19A 102.8(2) . . ?
C18A N3A N2A 110.27(19) . . ?
C18A N3A C20A 128.6(2) . . ?
N2A N3A C20A 120.84(19) . . ?
C21A N5A N4A 101.9(2) . . ?
C22A N4A N5A 110.36(19) . . ?
C22A N4A C20A 131.2(2) . . ?
N5A N4A C20A 118.17(19) . . ?
C18 N1 C19 102.9(2) . . ?
C22 N4 N5 110.33(19) . . ?
C22 N4 C20 129.4(2) . . ?
N5 N4 C20 120.21(19) . . ?
C22A N6A C21A 103.1(2) . . ?
C21 N5 N4 101.8(2) . . ?
C22 N6 C21 102.9(2) . . ?
N2A C19A N1A 115.8(2) . . ?
N2A C19A H19A 122.1 . . ?
N1A C19A H19A 122.1 . . ?
C28 C23 C24 119.5(2) . . ?
C28 C23 P2 120.92(19) . . ?
C24 C23 P2 119.5(2) . . ?
C30 C29 C34 118.5(2) . . ?
C30 C29 P2 120.22(18) . . ?
C34 C29 P2 121.03(19) . . ?
C33 C34 C29 120.6(2) . . ?
C33 C34 H34 119.7 . . ?
C29 C34 H34 119.7 . . ?
C7A C6A C11A 118.8(2) . . ?
C7A C6A P1A 121.15(19) . . ?
C11A C6A P1A 119.8(2) . . ?
C8 C7 C6 119.9(2) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C11 C6 C7 119.2(2) . . ?
C11 C6 P1 122.61(18) . . ?
C7 C6 P1 118.06(18) . . ?
C23 C28 C27 119.5(3) . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 119.6(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
N6 C22 N4 109.3(2) . . ?
N6 C22 P2 129.31(18) . . ?
N4 C22 P2 120.92(17) . . ?
N1A C18A N3A 109.4(2) . . ?
N1A C18A P1A 128.87(18) . . ?
N3A C18A P1A 121.64(18) . . ?
N5A C21A N6A 115.2(2) . . ?
N5A C21A H21A 122.4 . . ?
N6A C21A H21A 122.4 . . ?
N1 C18 N3 109.4(2) . . ?
N1 C18 P1 123.78(18) . . ?
N3 C18 P1 126.79(17) . . ?
C13A C12A C17A 118.9(2) . . ?
C13A C12A P1A 121.8(2) . . ?
C17A C12A P1A 119.3(2) . . ?
C14A C13A C12A 120.6(3) . . ?
C14A C13A H13A 119.7 . . ?
C12A C13A H13A 119.7 . . ?
C31A C30A C29A 120.7(3) . . ?
C31A C30A H30A 119.6 . . ?
C29A C30A H30A 119.6 . . ?
C32 C33 C34 120.2(2) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C28A C23A C24A 119.2(2) . . ?
C28A C23A P2A 123.0(2) . . ?
C24A C23A P2A 117.76(19) . . ?
C26A C25A C24A 120.4(3) . . ?
C26A C25A H25A 119.8 . . ?
C24A C25A H25A 119.8 . . ?
C29 C30 C31 121.0(2) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C25A C24A C23A 120.1(3) . . ?
C25A C24A H24A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C10A C9A C8A 120.0(3) . . ?
C10A C9A H9A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C15 C16 C17 120.6(3) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C27A C28A C23A 120.1(3) . . ?
C27A C28A H28A 119.9 . . ?
C23A C28A H28A 119.9 . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C6 C11 C10 120.6(2) . . ?
C6 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C34A C29A C30A 118.7(2) . . ?
C34A C29A P2A 122.7(2) . . ?
C30A C29A P2A 118.00(19) . . ?
C12 C17 C16 120.3(3) . . ?
C12 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
N4 C20 N3 112.01(19) . . ?
N4 C20 H20A 109.2 . . ?
N3 C20 H20A 109.2 . . ?
N4 C20 H20B 109.2 . . ?
N3 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C9 C8 C7 120.3(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C9A C10A C11A 120.2(3) . . ?
C9A C10A H10A 119.9 . . ?
C11A C10A H10A 119.9 . . ?
C32A C31A C30A 120.1(3) . . ?
C32A C31A H31A 120.0 . . ?
C30A C31A H31A 120.0 . . ?
N2 C19 N1 115.7(2) . . ?
N2 C19 H19 122.2 . . ?
N1 C19 H19 122.2 . . ?
C15A C16A C17A 120.3(3) . . ?
C15A C16A H16A 119.8 . . ?
C17A C16A H16A 119.8 . . ?
C10A C11A C6A 120.3(3) . . ?
C10A C11A H11A 119.9 . . ?
C6A C11A H11A 119.9 . . ?
C25 C24 C23 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C15A C14A C13A 119.8(3) . . ?
C15A C14A H14A 120.1 . . ?
C13A C14A H14A 120.1 . . ?
C26 C27 C28 120.6(3) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C16 C15 C14 119.6(2) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C27A C26A C25A 119.5(2) . . ?
C27A C26A H26A 120.3 . . ?
C25A C26A H26A 120.3 . . ?
C8A C7A C6A 120.2(3) . . ?
C8A C7A H7A 119.9 . . ?
C6A C7A H7A 119.9 . . ?
C17 C12 C13 118.5(2) . . ?
C17 C12 P1 123.73(19) . . ?
C13 C12 P1 117.67(19) . . ?
C32 C31 C30 119.8(3) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
N5 C21 N6 115.7(2) . . ?
N5 C21 H21 122.2 . . ?
N6 C21 H21 122.2 . . ?
C9A C8A C7A 120.5(3) . . ?
C9A C8A H8A 119.8 . . ?
C7A C8A H8A 119.8 . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C16A C17A C12A 120.0(3) . . ?
C16A C17A H17A 120.0 . . ?
C12A C17A H17A 120.0 . . ?
C2 C1 C5 108.9(2) . . ?
C2 C1 Ru1 71.25(14) . . ?
C5 C1 Ru1 71.35(14) . . ?
C2 C1 H1 125.6 . . ?
C5 C1 H1 125.6 . . ?
Ru1 C1 H1 123.5 . . ?
N3A C20A N4A 111.8(2) . . ?
N3A C20A H20C 109.3 . . ?
N4A C20A H20C 109.3 . . ?
N3A C20A H20D 109.3 . . ?
N4A C20A H20D 109.3 . . ?
H20C C20A H20D 107.9 . . ?
C16A C15A C14A 120.3(3) . . ?
C16A C15A H15A 119.9 . . ?
C14A C15A H15A 119.9 . . ?
C4 C5 C1 107.0(2) . . ?
C4 C5 Ru1 70.63(14) . . ?
C1 C5 Ru1 71.19(14) . . ?
C4 C5 H5 126.5 . . ?
C1 C5 H5 126.5 . . ?
Ru1 C5 H5 123.4 . . ?
N6A C22A N4A 109.4(2) . . ?
N6A C22A P2A 123.76(18) . . ?
N4A C22A P2A 126.77(17) . . ?
C31A C32A C33A 119.9(3) . . ?
C31A C32A H32A 120.1 . . ?
C33A C32A H32A 120.1 . . ?
C33A C34A C29A 120.3(3) . . ?
C33A C34A H34A 119.8 . . ?
C29A C34A H34A 119.8 . . ?
C1 C2 C3 107.8(2) . . ?
C1 C2 Ru1 71.77(14) . . ?
C3 C2 Ru1 69.95(14) . . ?
C1 C2 H2 126.1 . . ?
C3 C2 H2 126.1 . . ?
Ru1 C2 H2 123.8 . . ?
C26A C27A C28A 120.7(3) . . ?
C26A C27A H27A 119.6 . . ?
C28A C27A H27A 119.6 . . ?
C5 C4 C3 109.1(2) . . ?
C5 C4 Ru1 72.11(14) . . ?
C3 C4 Ru1 70.49(14) . . ?
C5 C4 H4 125.5 . . ?
C3 C4 H4 125.5 . . ?
Ru1 C4 H4 123.5 . . ?
Cl2 C35 Cl3 111.68(16) . . ?
Cl2 C35 H35A 109.3 . . ?
Cl3 C35 H35A 109.3 . . ?
Cl2 C35 H35B 109.3 . . ?
Cl3 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 120.0(3) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C2A C3A C4A 106.8(2) . . ?
C2A C3A Ru1A 69.95(14) . . ?
C4A C3A Ru1A 71.24(15) . . ?
C2A C3A H3A 126.6 . . ?
C4A C3A H3A 126.6 . . ?
Ru1A C3A H3A 123.9 . . ?
C32A C33A C34A 120.3(3) . . ?
C32A C33A H33A 119.9 . . ?
C34A C33A H33A 119.9 . . ?
C2A C1A C5A 107.3(2) . . ?
C2A C1A Ru1A 71.17(15) . . ?
C5A C1A Ru1A 72.73(15) . . ?
C2A C1A H1A 126.3 . . ?
C5A C1A H1A 126.3 . . ?
Ru1A C1A H1A 121.5 . . ?
C3A C2A C1A 108.9(3) . . ?
C3A C2A Ru1A 72.58(15) . . ?
C1A C2A Ru1A 70.95(15) . . ?
C3A C2A H2A 125.6 . . ?
C1A C2A H2A 125.6 . . ?
Ru1A C2A H2A 122.6 . . ?
C4 C3 C2 107.2(2) . . ?
C4 C3 Ru1 71.80(14) . . ?
C2 C3 Ru1 72.05(14) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
Ru1 C3 H3 121.5 . . ?
C5A C4A C3A 109.1(3) . . ?
C5A C4A Ru1A 71.87(15) . . ?
C3A C4A Ru1A 71.40(15) . . ?
C5A C4A H4A 125.4 . . ?
C3A C4A H4A 125.4 . . ?
Ru1A C4A H4A 122.9 . . ?
C4A C5A C1A 107.8(2) . . ?
C4A C5A Ru1A 71.31(15) . . ?
C1A C5A Ru1A 69.51(14) . . ?
C4A C5A H5A 126.1 . . ?
C1A C5A H5A 126.1 . . ?
Ru1A C5A H5A 124.7 . . ?
Cl3A C35A Cl2A 111.05(19) . . ?
Cl3A C35A H35C 109.4 . . ?
Cl2A C35A H35C 109.4 . . ?
Cl3A C35A H35D 109.4 . . ?
Cl2A C35A H35D 109.4 . . ?
H35C C35A H35D 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 N3 N2 C19 0.3(2) . . . . ?
C20 N3 N2 C19 -178.1(2) . . . . ?
C19A N2A N3A C18A 1.1(3) . . . . ?
C19A N2A N3A C20A 175.3(2) . . . . ?
C21A N5A N4A C22A -0.8(3) . . . . ?
C21A N5A N4A C20A -175.5(2) . . . . ?
C22 N4 N5 C21 0.2(3) . . . . ?
C20 N4 N5 C21 177.8(2) . . . . ?
N3A N2A C19A N1A -1.0(3) . . . . ?
C18A N1A C19A N2A 0.4(3) . . . . ?
C22 P2 C23 C28 132.1(2) . . . . ?
C29 P2 C23 C28 -125.9(2) . . . . ?
Ru1 P2 C23 C28 1.9(2) . . . . ?
C22 P2 C23 C24 -45.6(2) . . . . ?
C29 P2 C23 C24 56.5(2) . . . . ?
Ru1 P2 C23 C24 -175.74(18) . . . . ?
C22 P2 C29 C30 134.6(2) . . . . ?
C23 P2 C29 C30 37.3(2) . . . . ?
Ru1 P2 C29 C30 -94.6(2) . . . . ?
C22 P2 C29 C34 -51.7(2) . . . . ?
C23 P2 C29 C34 -149.0(2) . . . . ?
Ru1 P2 C29 C34 79.1(2) . . . . ?
C30 C29 C34 C33 0.3(4) . . . . ?
P2 C29 C34 C33 -173.50(19) . . . . ?
C12A P1A C6A C7A -155.6(2) . . . . ?
C18A P1A C6A C7A -52.7(2) . . . . ?
Ru1A P1A C6A C7A 73.9(2) . . . . ?
C12A P1A C6A C11A 30.3(2) . . . . ?
C18A P1A C6A C11A 133.2(2) . . . . ?
Ru1A P1A C6A C11A -100.2(2) . . . . ?
C8 C7 C6 C11 0.2(4) . . . . ?
C8 C7 C6 P1 -176.53(19) . . . . ?
C12 P1 C6 C11 -1.4(2) . . . . ?
C18 P1 C6 C11 102.2(2) . . . . ?
Ru1 P1 C6 C11 -129.9(2) . . . . ?
C12 P1 C6 C7 175.21(19) . . . . ?
C18 P1 C6 C7 -81.1(2) . . . . ?
Ru1 P1 C6 C7 46.8(2) . . . . ?
C24 C23 C28 C27 0.0(4) . . . . ?
P2 C23 C28 C27 -177.7(2) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C21 N6 C22 N4 -0.1(3) . . . . ?
C21 N6 C22 P2 -172.2(2) . . . . ?
N5 N4 C22 N6 -0.1(3) . . . . ?
C20 N4 C22 N6 -177.4(2) . . . . ?
N5 N4 C22 P2 172.79(16) . . . . ?
C20 N4 C22 P2 -4.6(3) . . . . ?
C23 P2 C22 N6 100.0(2) . . . . ?
C29 P2 C22 N6 -3.3(2) . . . . ?
Ru1 P2 C22 N6 -129.8(2) . . . . ?
C23 P2 C22 N4 -71.3(2) . . . . ?
C29 P2 C22 N4 -174.60(19) . . . . ?
Ru1 P2 C22 N4 58.9(2) . . . . ?
C19A N1A C18A N3A 0.3(3) . . . . ?
C19A N1A C18A P1A 176.6(2) . . . . ?
N2A N3A C18A N1A -1.0(3) . . . . ?
C20A N3A C18A N1A -174.6(2) . . . . ?
N2A N3A C18A P1A -177.55(16) . . . . ?
C20A N3A C18A P1A 8.9(3) . . . . ?
C6A P1A C18A N1A 10.5(2) . . . . ?
C12A P1A C18A N1A 115.4(2) . . . . ?
Ru1A P1A C18A N1A -114.4(2) . . . . ?
C6A P1A C18A N3A -173.62(19) . . . . ?
C12A P1A C18A N3A -68.7(2) . . . . ?
Ru1A P1A C18A N3A 61.5(2) . . . . ?
N4A N5A C21A N6A -0.1(3) . . . . ?
C22A N6A C21A N5A 0.9(3) . . . . ?
C19 N1 C18 N3 -0.2(3) . . . . ?
C19 N1 C18 P1 -177.27(18) . . . . ?
N2 N3 C18 N1 -0.1(3) . . . . ?
C20 N3 C18 N1 178.1(2) . . . . ?
N2 N3 C18 P1 176.90(17) . . . . ?
C20 N3 C18 P1 -4.9(4) . . . . ?
C12 P1 C18 N1 90.5(2) . . . . ?
C6 P1 C18 N1 -16.0(2) . . . . ?
Ru1 P1 C18 N1 -138.46(17) . . . . ?
C12 P1 C18 N3 -86.1(2) . . . . ?
C6 P1 C18 N3 167.4(2) . . . . ?
Ru1 P1 C18 N3 44.9(2) . . . . ?
C6A P1A C12A C13A 82.1(2) . . . . ?
C18A P1A C12A C13A -22.1(2) . . . . ?
Ru1A P1A C12A C13A -150.62(17) . . . . ?
C6A P1A C12A C17A -96.3(2) . . . . ?
C18A P1A C12A C17A 159.49(19) . . . . ?
Ru1A P1A C12A C17A 31.0(2) . . . . ?
C17A C12A C13A C14A -1.7(4) . . . . ?
P1A C12A C13A C14A 179.95(19) . . . . ?
C29 C34 C33 C32 0.5(4) . . . . ?
C29A P2A C23A C28A 12.3(2) . . . . ?
C22A P2A C23A C28A 116.6(2) . . . . ?
Ru1A P2A C23A C28A -117.0(2) . . . . ?
C29A P2A C23A C24A -168.3(2) . . . . ?
C22A P2A C23A C24A -64.1(2) . . . . ?
Ru1A P2A C23A C24A 62.4(2) . . . . ?
C34 C29 C30 C31 -0.8(4) . . . . ?
P2 C29 C30 C31 173.1(2) . . . . ?
C26A C25A C24A C23A 1.2(4) . . . . ?
C28A C23A C24A C25A -1.7(4) . . . . ?
P2A C23A C24A C25A 178.91(19) . . . . ?
C24A C23A C28A C27A 1.0(4) . . . . ?
P2A C23A C28A C27A -179.6(2) . . . . ?
C12 C13 C14 C15 1.2(4) . . . . ?
C7 C6 C11 C10 0.2(4) . . . . ?
P1 C6 C11 C10 176.8(2) . . . . ?
C9 C10 C11 C6 -0.7(4) . . . . ?
C31A C30A C29A C34A -2.0(4) . . . . ?
C31A C30A C29A P2A 169.4(2) . . . . ?
C23A P2A C29A C34A 78.1(2) . . . . ?
C22A P2A C29A C34A -22.0(2) . . . . ?
Ru1A P2A C29A C34A -158.82(19) . . . . ?
C23A P2A C29A C30A -92.9(2) . . . . ?
C22A P2A C29A C30A 166.99(19) . . . . ?
Ru1A P2A C29A C30A 30.2(2) . . . . ?
C15 C16 C17 C12 0.8(4) . . . . ?
C22 N4 C20 N3 -106.3(3) . . . . ?
N5 N4 C20 N3 76.6(3) . . . . ?
C18 N3 C20 N4 68.1(3) . . . . ?
N2 N3 C20 N4 -113.8(2) . . . . ?
C10 C9 C8 C7 -0.4(4) . . . . ?
C6 C7 C8 C9 -0.1(4) . . . . ?
C8A C9A C10A C11A -0.9(4) . . . . ?
C29A C30A C31A C32A 1.5(4) . . . . ?
N3 N2 C19 N1 -0.5(3) . . . . ?
C18 N1 C19 N2 0.4(3) . . . . ?
C9A C10A C11A C6A 0.8(4) . . . . ?
C7A C6A C11A C10A 0.1(4) . . . . ?
P1A C6A C11A C10A 174.3(2) . . . . ?
C28 C23 C24 C25 -0.1(4) . . . . ?
P2 C23 C24 C25 177.6(2) . . . . ?
C12A C13A C14A C15A 2.0(4) . . . . ?
C23 C28 C27 C26 0.2(4) . . . . ?
C17 C16 C15 C14 1.5(4) . . . . ?
C13 C14 C15 C16 -2.5(4) . . . . ?
C24A C25A C26A C27A 0.0(4) . . . . ?
C11A C6A C7A C8A -0.8(4) . . . . ?
P1A C6A C7A C8A -174.98(19) . . . . ?
C16 C17 C12 C13 -2.0(4) . . . . ?
C16 C17 C12 P1 174.88(19) . . . . ?
C14 C13 C12 C17 1.0(4) . . . . ?
C14 C13 C12 P1 -176.1(2) . . . . ?
C6 P1 C12 C17 101.8(2) . . . . ?
C18 P1 C12 C17 -0.1(2) . . . . ?
Ru1 P1 C12 C17 -132.80(18) . . . . ?
C6 P1 C12 C13 -81.2(2) . . . . ?
C18 P1 C12 C13 176.80(19) . . . . ?
Ru1 P1 C12 C13 44.1(2) . . . . ?
C29 C30 C31 C32 0.4(4) . . . . ?
N4 N5 C21 N6 -0.3(3) . . . . ?
C22 N6 C21 N5 0.2(3) . . . . ?
C10A C9A C8A C7A 0.1(4) . . . . ?
C6A C7A C8A C9A 0.8(4) . . . . ?
C34 C33 C32 C31 -0.8(4) . . . . ?
C30 C31 C32 C33 0.4(4) . . . . ?
C15A C16A C17A C12A 1.2(4) . . . . ?
C13A C12A C17A C16A 0.1(4) . . . . ?
P1A C12A C17A C16A 178.5(2) . . . . ?
C18A N3A C20A N4A -114.4(3) . . . . ?
N2A N3A C20A N4A 72.6(3) . . . . ?
C22A N4A C20A N3A 57.7(3) . . . . ?
N5A N4A C20A N3A -129.0(2) . . . . ?
C17A C16A C15A C14A -1.0(4) . . . . ?
C13A C14A C15A C16A -0.6(4) . . . . ?
C2 C1 C5 C4 0.2(3) . . . . ?
Ru1 C1 C5 C4 61.93(17) . . . . ?
C2 C1 C5 Ru1 -61.71(17) . . . . ?
C21A N6A C22A N4A -1.4(3) . . . . ?
C21A N6A C22A P2A 176.80(19) . . . . ?
N5A N4A C22A N6A 1.5(3) . . . . ?
C20A N4A C22A N6A 175.2(2) . . . . ?
N5A N4A C22A P2A -176.66(18) . . . . ?
C20A N4A C22A P2A -2.9(4) . . . . ?
C29A P2A C22A N6A 94.8(2) . . . . ?
C23A P2A C22A N6A -8.5(2) . . . . ?
Ru1A P2A C22A N6A -128.23(19) . . . . ?
C29A P2A C22A N4A -87.3(2) . . . . ?
C23A P2A C22A N4A 169.4(2) . . . . ?
Ru1A P2A C22A N4A 49.7(2) . . . . ?
C30A C31A C32A C33A 0.3(4) . . . . ?
C30A C29A C34A C33A 0.8(4) . . . . ?
P2A C29A C34A C33A -170.2(2) . . . . ?
C5 C1 C2 C3 0.8(3) . . . . ?
Ru1 C1 C2 C3 -60.98(17) . . . . ?
C5 C1 C2 Ru1 61.77(17) . . . . ?
C25A C26A C27A C28A -0.7(4) . . . . ?
C23A C28A C27A C26A 0.2(4) . . . . ?
C1 C5 C4 C3 -1.2(3) . . . . ?
Ru1 C5 C4 C3 61.13(17) . . . . ?
C1 C5 C4 Ru1 -62.30(17) . . . . ?
C23 C24 C25 C26 0.0(5) . . . . ?
C24 C25 C26 C27 0.1(5) . . . . ?
C28 C27 C26 C25 -0.2(4) . . . . ?
C31A C32A C33A C34A -1.5(5) . . . . ?
C29A C34A C33A C32A 1.0(5) . . . . ?
C4A C3A C2A C1A 0.0(3) . . . . ?
Ru1A C3A C2A C1A 62.04(18) . . . . ?
C4A C3A C2A Ru1A -62.09(18) . . . . ?
C5A C1A C2A C3A 1.1(3) . . . . ?
Ru1A C1A C2A C3A -63.07(18) . . . . ?
C5A C1A C2A Ru1A 64.21(18) . . . . ?
C5 C4 C3 C2 1.7(3) . . . . ?
Ru1 C4 C3 C2 63.80(17) . . . . ?
C5 C4 C3 Ru1 -62.15(17) . . . . ?
C1 C2 C3 C4 -1.5(3) . . . . ?
Ru1 C2 C3 C4 -63.64(17) . . . . ?
C1 C2 C3 Ru1 62.15(17) . . . . ?
C2A C3A C4A C5A -1.1(3) . . . . ?
Ru1A C3A C4A C5A -62.34(19) . . . . ?
C2A C3A C4A Ru1A 61.24(18) . . . . ?
C3A C4A C5A C1A 1.8(3) . . . . ?
Ru1A C4A C5A C1A -60.23(18) . . . . ?
C3A C4A C5A Ru1A 62.04(19) . . . . ?
C2A C1A C5A C4A -1.8(3) . . . . ?
Ru1A C1A C5A C4A 61.38(19) . . . . ?
C2A C1A C5A Ru1A -63.19(17) . . . . ?

_refine_diff_density_max         0.381
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.086

