# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C28 H23 Br Cl N3 Pd'

_chemical_formula_weight         623.25



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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   P2(1)/c



loop_

_symmetry_equiv_pos_as_xyz




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



_cell_length_a                   10.6120(14)

_cell_length_b                   10.1775(13)

_cell_length_c                   24.139(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 100.7810(10)

_cell_angle_gamma                90.00

_cell_volume                     2561.1(6)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    8183

_cell_measurement_theta_min      2.64

_cell_measurement_theta_max      27.93



_exptl_crystal_description       block

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.33

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.17

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.616

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1240

_exptl_absorpt_coefficient_mu    2.410

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.5035

_exptl_absorpt_correction_T_max  0.6847

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            17818

_diffrn_reflns_av_R_equivalents  0.0202

_diffrn_reflns_av_sigmaI/netI    0.0184

_diffrn_reflns_limit_h_min       -12

_diffrn_reflns_limit_h_max       12

_diffrn_reflns_limit_k_min       -12

_diffrn_reflns_limit_k_max       12

_diffrn_reflns_limit_l_min       -29

_diffrn_reflns_limit_l_max       28

_diffrn_reflns_theta_min         2.35

_diffrn_reflns_theta_max         25.50

_reflns_number_total             4757

_reflns_number_gt                4017

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0256P)²+1.2802P] 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         4757

_refine_ls_number_parameters     309

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0300

_refine_ls_R_factor_gt           0.0219

_refine_ls_wR_factor_ref         0.0553

_refine_ls_wR_factor_gt          0.0518

_refine_ls_goodness_of_fit_ref   1.017

_refine_ls_restrained_S_all      1.017

_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

























































Pd1 Pd 0.212070(15) 0.246921(15) 0.114419(7) 0.03265(6) Uani 1 1 d . . .
Br1 Br 0.35438(3) 0.64055(3) -0.042317(13) 0.07189(10) Uani 1 1 d . . .
Cl1 Cl 0.22015(6) 0.12921(6) 0.20214(3) 0.05285(16) Uani 1 1 d . . .
N1 N 0.49734(17) 0.27201(17) 0.15582(7) 0.0346(4) Uani 1 1 d . . .
N2 N 0.39744(16) 0.44779(17) 0.17176(7) 0.0349(4) Uani 1 1 d . . .
N3 N 0.03813(18) 0.17141(19) 0.07364(9) 0.0439(5) Uani 1 1 d . . .
C1 C 0.3790(2) 0.3265(2) 0.14752(8) 0.0315(4) Uani 1 1 d . . .
C2 C 0.5877(2) 0.3576(2) 0.18563(10) 0.0438(6) Uani 1 1 d . . .
H2 H 0.6751 0.3415 0.1967 0.053 Uiso 1 1 calc R . .
C3 C 0.5263(2) 0.4665(2) 0.19542(10) 0.0430(6) Uani 1 1 d . . .
H3 H 0.5624 0.5409 0.2144 0.052 Uiso 1 1 calc R . .
C4 C 0.5257(2) 0.1400(2) 0.14046(9) 0.0352(5) Uani 1 1 d . . .
C5 C 0.4747(2) 0.0886(2) 0.08837(10) 0.0453(6) Uani 1 1 d . . .
H5 H 0.4204 0.1390 0.0619 0.054 Uiso 1 1 calc R . .
C6 C 0.5050(2) -0.0393(2) 0.07564(11) 0.0493(6) Uani 1 1 d . . .
H6 H 0.4698 -0.0738 0.0405 0.059 Uiso 1 1 calc R . .
C7 C 0.5856(2) -0.1167(2) 0.11362(11) 0.0458(6) Uani 1 1 d . . .
C8 C 0.6362(3) -0.0628(3) 0.16532(11) 0.0583(7) Uani 1 1 d . . .
H8 H 0.6906 -0.1131 0.1918 0.070 Uiso 1 1 calc R . .
C9 C 0.6076(3) 0.0646(3) 0.17867(10) 0.0537(7) Uani 1 1 d . . .
H9 H 0.6440 0.0994 0.2136 0.064 Uiso 1 1 calc R . .
C10 C 0.6210(3) -0.2545(3) 0.09849(14) 0.0640(8) Uani 1 1 d . . .
H10A H 0.5448 -0.3014 0.0819 0.096 Uiso 1 1 calc R . .
H10B H 0.6625 -0.2994 0.1319 0.096 Uiso 1 1 calc R . .
H10C H 0.6782 -0.2501 0.0721 0.096 Uiso 1 1 calc R . .
C11 C 0.2973(2) 0.5394(2) 0.17688(8) 0.0340(5) Uani 1 1 d . . .
C12 C 0.3145(2) 0.6720(2) 0.16823(10) 0.0418(5) Uani 1 1 d . . .
H12 H 0.3878 0.7013 0.1561 0.050 Uiso 1 1 calc R . .
C13 C 0.2218(3) 0.7610(2) 0.17776(10) 0.0468(6) Uani 1 1 d . . .
H13 H 0.2341 0.8502 0.1725 0.056 Uiso 1 1 calc R . .
C14 C 0.1110(3) 0.7187(2) 0.19508(10) 0.0461(6) Uani 1 1 d . . .
C15 C 0.0953(2) 0.5852(2) 0.20262(10) 0.0422(5) Uani 1 1 d . . .
H15 H 0.0211 0.5554 0.2138 0.051 Uiso 1 1 calc R . .
C16 C 0.1870(2) 0.4955(2) 0.19401(9) 0.0381(5) Uani 1 1 d . . .
H16 H 0.1749 0.4063 0.1996 0.046 Uiso 1 1 calc R . .
C17 C 0.0096(3) 0.8143(3) 0.20596(16) 0.0804(10) Uani 1 1 d . . .
H17A H -0.0583 0.8179 0.1735 0.121 Uiso 1 1 calc R . .
H17B H 0.0469 0.9000 0.2131 0.121 Uiso 1 1 calc R . .
H17C H -0.0243 0.7858 0.2381 0.121 Uiso 1 1 calc R . .
C18 C 0.0004(2) 0.2141(2) 0.02002(11) 0.0452(6) Uani 1 1 d . . .
C19 C -0.1070(3) 0.1580(3) -0.01373(14) 0.0655(8) Uani 1 1 d . . .
H19 H -0.1333 0.1864 -0.0507 0.079 Uiso 1 1 calc R . .
C20 C -0.1735(3) 0.0613(3) 0.00757(17) 0.0807(10) Uani 1 1 d . . .
H20 H -0.2435 0.0217 -0.0153 0.097 Uiso 1 1 calc R . .
C21 C -0.1371(3) 0.0230(3) 0.06241(18) 0.0796(10) Uani 1 1 d . . .
H21 H -0.1836 -0.0403 0.0778 0.095 Uiso 1 1 calc R . .
C22 C -0.0301(3) 0.0800(3) 0.09458(14) 0.0629(7) Uani 1 1 d . . .
H22 H -0.0047 0.0540 0.1319 0.076 Uiso 1 1 calc R . .
C23 C 0.0825(2) 0.3159(2) 0.00330(9) 0.0406(5) Uani 1 1 d . . .
C24 C 0.1949(2) 0.3473(2) 0.04266(9) 0.0351(5) Uani 1 1 d . . .
C25 C 0.2745(2) 0.4449(2) 0.02788(9) 0.0391(5) Uani 1 1 d . . .
H25 H 0.3495 0.4674 0.0526 0.047 Uiso 1 1 calc R . .
C26 C 0.2422(3) 0.5086(2) -0.02343(10) 0.0464(6) Uani 1 1 d . . .
C27 C 0.1318(3) 0.4800(3) -0.06156(10) 0.0550(7) Uani 1 1 d . . .
H27 H 0.1115 0.5250 -0.0956 0.066 Uiso 1 1 calc R . .
C28 C 0.0526(3) 0.3836(3) -0.04804(11) 0.0544(7) Uani 1 1 d . . .
H28 H -0.0221 0.3627 -0.0733 0.065 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






























































Pd1 C1 1.976(2) . ?
Pd1 C24 1.990(2) . ?
Pd1 N3 2.0705(18) . ?
Pd1 Cl1 2.4205(7) . ?
Br1 C26 1.906(3) . ?
N1 C1 1.353(3) . ?
N1 C2 1.392(3) . ?
N1 C4 1.440(3) . ?
N2 C1 1.364(3) . ?
N2 C3 1.393(3) . ?
N2 C11 1.437(3) . ?
N3 C22 1.335(3) . ?
N3 C18 1.353(3) . ?
C2 C3 1.329(3) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.376(3) . ?
C4 C9 1.377(3) . ?
C5 C6 1.389(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.378(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(4) . ?
C7 C10 1.514(3) . ?
C8 C9 1.383(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.383(3) . ?
C11 C16 1.386(3) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(3) . ?
C14 C17 1.510(4) . ?
C15 C16 1.378(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.393(3) . ?
C18 C23 1.459(4) . ?
C19 C20 1.366(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.378(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C28 1.401(3) . ?
C23 C24 1.415(3) . ?
C24 C25 1.393(3) . ?
C25 C26 1.383(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.379(4) . ?
C27 C28 1.370(4) . ?
C27 H27 0.9300 . ?
C28 H28 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









































































































C1 Pd1 C24 94.06(8) . . ?
C1 Pd1 N3 175.30(8) . . ?
C24 Pd1 N3 81.27(8) . . ?
C1 Pd1 Cl1 88.10(6) . . ?
C24 Pd1 Cl1 176.55(6) . . ?
N3 Pd1 Cl1 96.59(6) . . ?
C1 N1 C2 110.52(18) . . ?
C1 N1 C4 125.25(18) . . ?
C2 N1 C4 124.04(18) . . ?
C1 N2 C3 110.52(18) . . ?
C1 N2 C11 125.10(17) . . ?
C3 N2 C11 124.16(18) . . ?
C22 N3 C18 120.1(2) . . ?
C22 N3 Pd1 125.24(18) . . ?
C18 N3 Pd1 114.44(16) . . ?
N1 C1 N2 104.64(17) . . ?
N1 C1 Pd1 128.96(15) . . ?
N2 C1 Pd1 126.17(15) . . ?
C3 C2 N1 107.46(19) . . ?
C3 C2 H2 126.3 . . ?
N1 C2 H2 126.3 . . ?
C2 C3 N2 106.8(2) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
C5 C4 C9 119.4(2) . . ?
C5 C4 N1 121.64(19) . . ?
C9 C4 N1 118.9(2) . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 121.9(2) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C8 C7 C6 117.6(2) . . ?
C8 C7 C10 121.0(2) . . ?
C6 C7 C10 121.3(2) . . ?
C7 C8 C9 121.3(2) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C8 120.3(2) . . ?
C4 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 120.2(2) . . ?
C12 C11 N2 120.0(2) . . ?
C16 C11 N2 119.73(19) . . ?
C11 C12 C13 119.6(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 121.0(2) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 118.2(2) . . ?
C15 C14 C17 120.1(2) . . ?
C13 C14 C17 121.6(2) . . ?
C16 C15 C14 121.7(2) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C11 119.3(2) . . ?
C15 C16 H16 120.3 . . ?
C11 C16 H16 120.3 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 119.4(3) . . ?
N3 C18 C23 114.1(2) . . ?
C19 C18 C23 126.5(3) . . ?
C20 C19 C18 119.9(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 118.7(3) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
N3 C22 C21 121.9(3) . . ?
N3 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C28 C23 C24 120.4(2) . . ?
C28 C23 C18 123.1(2) . . ?
C24 C23 C18 116.5(2) . . ?
C25 C24 C23 117.7(2) . . ?
C25 C24 Pd1 128.89(16) . . ?
C23 C24 Pd1 113.40(16) . . ?
C26 C25 C24 120.2(2) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C25 122.4(2) . . ?
C27 C26 Br1 118.69(19) . . ?
C25 C26 Br1 118.91(19) . . ?
C28 C27 C26 118.3(2) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C27 C28 C23 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?



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























































































C1 Pd1 N3 C22 172.3(9) . . . . ?
C24 Pd1 N3 C22 178.8(2) . . . . ?
Cl1 Pd1 N3 C22 -3.9(2) . . . . ?
C1 Pd1 N3 C18 -2.3(11) . . . . ?
C24 Pd1 N3 C18 4.23(17) . . . . ?
Cl1 Pd1 N3 C18 -178.50(16) . . . . ?
C2 N1 C1 N2 1.0(2) . . . . ?
C4 N1 C1 N2 176.05(18) . . . . ?
C2 N1 C1 Pd1 -173.89(16) . . . . ?
C4 N1 C1 Pd1 1.2(3) . . . . ?
C3 N2 C1 N1 -0.8(2) . . . . ?
C11 N2 C1 N1 -175.59(18) . . . . ?
C3 N2 C1 Pd1 174.23(15) . . . . ?
C11 N2 C1 Pd1 -0.6(3) . . . . ?
C24 Pd1 C1 N1 -106.96(19) . . . . ?
N3 Pd1 C1 N1 -100.5(10) . . . . ?
Cl1 Pd1 C1 N1 75.73(18) . . . . ?
C24 Pd1 C1 N2 79.22(18) . . . . ?
N3 Pd1 C1 N2 85.7(10) . . . . ?
Cl1 Pd1 C1 N2 -98.08(17) . . . . ?
C1 N1 C2 C3 -0.8(3) . . . . ?
C4 N1 C2 C3 -175.9(2) . . . . ?
N1 C2 C3 N2 0.2(3) . . . . ?
C1 N2 C3 C2 0.4(3) . . . . ?
C11 N2 C3 C2 175.2(2) . . . . ?
C1 N1 C4 C5 46.6(3) . . . . ?
C2 N1 C4 C5 -138.9(2) . . . . ?
C1 N1 C4 C9 -134.5(2) . . . . ?
C2 N1 C4 C9 40.0(3) . . . . ?
C9 C4 C5 C6 1.1(4) . . . . ?
N1 C4 C5 C6 -180.0(2) . . . . ?
C4 C5 C6 C7 -0.4(4) . . . . ?
C5 C6 C7 C8 0.0(4) . . . . ?
C5 C6 C7 C10 -178.1(2) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C10 C7 C8 C9 177.8(3) . . . . ?
C5 C4 C9 C8 -1.4(4) . . . . ?
N1 C4 C9 C8 179.6(2) . . . . ?
C7 C8 C9 C4 1.0(4) . . . . ?
C1 N2 C11 C12 -140.0(2) . . . . ?
C3 N2 C11 C12 45.9(3) . . . . ?
C1 N2 C11 C16 44.1(3) . . . . ?
C3 N2 C11 C16 -130.0(2) . . . . ?
C16 C11 C12 C13 1.1(3) . . . . ?
N2 C11 C12 C13 -174.7(2) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 0.0(4) . . . . ?
C12 C13 C14 C17 179.6(3) . . . . ?
C13 C14 C15 C16 0.8(4) . . . . ?
C17 C14 C15 C16 -178.9(3) . . . . ?
C14 C15 C16 C11 -0.6(3) . . . . ?
C12 C11 C16 C15 -0.4(3) . . . . ?
N2 C11 C16 C15 175.50(19) . . . . ?
C22 N3 C18 C19 -2.6(4) . . . . ?
Pd1 N3 C18 C19 172.32(19) . . . . ?
C22 N3 C18 C23 178.8(2) . . . . ?
Pd1 N3 C18 C23 -6.3(3) . . . . ?
N3 C18 C19 C20 0.4(4) . . . . ?
C23 C18 C19 C20 178.8(3) . . . . ?
C18 C19 C20 C21 2.2(5) . . . . ?
C19 C20 C21 C22 -2.5(5) . . . . ?
C18 N3 C22 C21 2.3(4) . . . . ?
Pd1 N3 C22 C21 -172.0(2) . . . . ?
C20 C21 C22 N3 0.2(5) . . . . ?
N3 C18 C23 C28 -172.7(2) . . . . ?
C19 C18 C23 C28 8.8(4) . . . . ?
N3 C18 C23 C24 5.5(3) . . . . ?
C19 C18 C23 C24 -173.0(2) . . . . ?
C28 C23 C24 C25 -1.3(3) . . . . ?
C18 C23 C24 C25 -179.5(2) . . . . ?
C28 C23 C24 Pd1 176.30(18) . . . . ?
C18 C23 C24 Pd1 -2.0(3) . . . . ?
C1 Pd1 C24 C25 -4.4(2) . . . . ?
N3 Pd1 C24 C25 176.2(2) . . . . ?
Cl1 Pd1 C24 C25 124.3(10) . . . . ?
C1 Pd1 C24 C23 178.36(16) . . . . ?
N3 Pd1 C24 C23 -1.10(16) . . . . ?
Cl1 Pd1 C24 C23 -53.0(11) . . . . ?
C23 C24 C25 C26 0.7(3) . . . . ?
Pd1 C24 C25 C26 -176.49(17) . . . . ?
C24 C25 C26 C27 0.4(4) . . . . ?
C24 C25 C26 Br1 -179.51(16) . . . . ?
C25 C26 C27 C28 -0.9(4) . . . . ?
Br1 C26 C27 C28 179.02(19) . . . . ?
C26 C27 C28 C23 0.3(4) . . . . ?
C24 C23 C28 C27 0.8(4) . . . . ?
C18 C23 C28 C27 179.0(2) . . . . ?



_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.305

_refine_diff_density_min         -0.284

_refine_diff_density_rms         0.047

_database_code_depnum_ccdc_archive 'CCDC 981473'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dd



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C28.50 H24 Br Cl2 N3 O2 Pd'

_chemical_formula_weight         697.72



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source














C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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



loop_

_symmetry_equiv_pos_as_xyz


'x, y, z'
'-x, -y, -z'



_cell_length_a                   10.819(3)

_cell_length_b                   11.915(3)

_cell_length_c                   12.495(4)

_cell_angle_alpha                92.324(3)

_cell_angle_beta                 101.450(3)

_cell_angle_gamma                113.413(3)

_cell_volume                     1435.8(7)

_cell_formula_units_Z            2

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    5789

_cell_measurement_theta_min      2.37

_cell_measurement_theta_max      28.09



_exptl_crystal_description       block

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.41

_exptl_crystal_size_mid          0.30

_exptl_crystal_size_min          0.19

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.614

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             694

_exptl_absorpt_coefficient_mu    2.254

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.4584

_exptl_absorpt_correction_T_max  0.6740

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            10713

_diffrn_reflns_av_R_equivalents  0.0137

_diffrn_reflns_av_sigmaI/netI    0.0210

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       13

_diffrn_reflns_limit_k_min       -14

_diffrn_reflns_limit_k_max       14

_diffrn_reflns_limit_l_min       -15

_diffrn_reflns_limit_l_max       15

_diffrn_reflns_theta_min         2.59

_diffrn_reflns_theta_max         25.50

_reflns_number_total             5296

_reflns_number_gt                4704

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0501P)²+0.9640P] 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         5296

_refine_ls_number_parameters     364

_refine_ls_number_restraints     29

_refine_ls_R_factor_all          0.0355

_refine_ls_R_factor_gt           0.0296

_refine_ls_wR_factor_ref         0.0850

_refine_ls_wR_factor_gt          0.0808

_refine_ls_goodness_of_fit_ref   1.023

_refine_ls_restrained_S_all      1.046

_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_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group





































































C29 C 0.547(2) 0.9550(15) 0.5709(15) 0.206(9) Uani 0.178(3) 1 d PDU A -1
H29A H 0.6051 1.0010 0.6415 0.247 Uiso 0.178(3) 1 calc PR A -1
H29B H 0.5786 0.8925 0.5527 0.247 Uiso 0.178(3) 1 calc PR A -1
Cl4 Cl 0.573(2) 1.0580(19) 0.4695(19) 0.184(4) Uani 0.178(3) 1 d PDU A -1
Cl3 Cl 0.3729(18) 0.8788(15) 0.5858(14) 0.186(3) Uani 0.178(3) 1 d PDU A -1
Cl4' Cl 0.5000(17) 0.9973(14) 0.5316(12) 0.184(4) Uani 0.322(3) 1 d PD A -2
Cl3' Cl 0.2905(10) 0.8406(8) 0.6445(7) 0.186(3) Uani 0.322(3) 1 d PD A -2
C29' C 0.4616(14) 0.8968(17) 0.6337(15) 0.206(9) Uani 0.322(3) 1 d PD A -2
H29C H 0.4833 0.8275 0.6168 0.247 Uiso 0.322(3) 1 calc PR A -2
H29D H 0.5213 0.9407 0.7045 0.247 Uiso 0.322(3) 1 calc PR A -2
Pd1 Pd 0.76633(2) 0.78947(2) 0.686661(17) 0.03394(9) Uani 1 1 d . . .
Br1 Br 0.32558(5) 0.42225(4) 0.86289(4) 0.07561(15) Uani 1 1 d . . .
Cl1 Cl 0.98514(8) 0.95841(8) 0.68563(7) 0.0507(2) Uani 1 1 d . . .
O1 O 0.9568(3) 0.3552(2) 0.6225(2) 0.0670(7) Uani 1 1 d . . .
O2 O 0.6213(4) 1.2084(3) 0.9523(2) 0.0809(9) Uani 1 1 d . . .
N1 N 0.6792(3) 0.7762(2) 0.5208(2) 0.0392(6) Uani 1 1 d . . .
N2 N 0.8945(3) 0.7102(2) 0.8845(2) 0.0407(6) Uani 1 1 d . . .
N3 N 0.8392(3) 0.8549(2) 0.9374(2) 0.0386(5) Uani 1 1 d . . .
C1 C 0.7413(4) 0.8411(3) 0.4470(3) 0.0480(8) Uani 1 1 d . . .
H1 H 0.8332 0.8979 0.4701 0.058 Uiso 1 1 calc R . .
C2 C 0.6740(4) 0.8266(4) 0.3379(3) 0.0601(10) Uani 1 1 d . . .
H2 H 0.7196 0.8733 0.2885 0.072 Uiso 1 1 calc R . .
C3 C 0.5387(4) 0.7423(4) 0.3035(3) 0.0614(10) Uani 1 1 d . . .
H3 H 0.4913 0.7313 0.2304 0.074 Uiso 1 1 calc R . .
C4 C 0.4735(4) 0.6737(4) 0.3789(3) 0.0534(9) Uani 1 1 d . . .
H4 H 0.3820 0.6161 0.3566 0.064 Uiso 1 1 calc R . .
C5 C 0.5452(3) 0.6913(3) 0.4875(3) 0.0413(7) Uani 1 1 d . . .
C6 C 0.4890(3) 0.6257(3) 0.5761(3) 0.0413(7) Uani 1 1 d . . .
C7 C 0.5803(3) 0.6565(3) 0.6814(2) 0.0371(6) Uani 1 1 d . . .
C8 C 0.5290(3) 0.5950(3) 0.7667(3) 0.0446(7) Uani 1 1 d . . .
H8 H 0.5863 0.6125 0.8370 0.053 Uiso 1 1 calc R . .
C9 C 0.3933(4) 0.5083(3) 0.7469(3) 0.0515(8) Uani 1 1 d . . .
C10 C 0.3039(4) 0.4786(4) 0.6441(3) 0.0593(9) Uani 1 1 d . . .
H10 H 0.2127 0.4207 0.6328 0.071 Uiso 1 1 calc R . .
C11 C 0.3534(3) 0.5373(3) 0.5588(3) 0.0541(9) Uani 1 1 d . . .
H11 H 0.2953 0.5174 0.4887 0.065 Uiso 1 1 calc R . .
C12 C 0.9106(3) 0.6178(3) 0.8180(3) 0.0428(7) Uani 1 1 d . . .
C13 C 0.9711(3) 0.6475(3) 0.7292(3) 0.0481(8) Uani 1 1 d . . .
H13 H 1.0025 0.7280 0.7124 0.058 Uiso 1 1 calc R . .
C14 C 0.9848(4) 0.5577(3) 0.6660(3) 0.0543(8) Uani 1 1 d . . .
H14 H 1.0238 0.5773 0.6056 0.065 Uiso 1 1 calc R . .
C15 C 0.9400(3) 0.4370(3) 0.6922(3) 0.0517(8) Uani 1 1 d . . .
C16 C 0.8816(4) 0.4079(3) 0.7815(3) 0.0538(9) Uani 1 1 d . . .
H16 H 0.8530 0.3281 0.7998 0.065 Uiso 1 1 calc R . .
C17 C 0.8657(4) 0.4981(3) 0.8440(3) 0.0501(8) Uani 1 1 d . . .
H17 H 0.8248 0.4782 0.9035 0.060 Uiso 1 1 calc R . .
C18 C 0.9347(6) 0.2358(4) 0.6545(5) 0.0888(15) Uani 1 1 d . . .
H18A H 0.9910 0.2451 0.7269 0.133 Uiso 1 1 calc R . .
H18B H 0.9596 0.1911 0.6032 0.133 Uiso 1 1 calc R . .
H18C H 0.8389 0.1913 0.6548 0.133 Uiso 1 1 calc R . .
C19 C 0.8348(3) 0.7858(3) 0.8452(2) 0.0364(6) Uani 1 1 d . . .
C20 C 0.9358(4) 0.7323(3) 0.9987(3) 0.0511(8) Uani 1 1 d . . .
H20 H 0.9789 0.6919 1.0439 0.061 Uiso 1 1 calc R . .
C21 C 0.9027(3) 0.8217(3) 1.0316(3) 0.0486(8) Uani 1 1 d . . .
H21 H 0.9187 0.8559 1.1040 0.058 Uiso 1 1 calc R . .
C22 C 0.7826(3) 0.9455(3) 0.9416(2) 0.0411(7) Uani 1 1 d . . .
C23 C 0.7410(4) 0.9923(3) 0.8485(3) 0.0537(9) Uani 1 1 d . . .
H23 H 0.7493 0.9651 0.7805 0.064 Uiso 1 1 calc R . .
C24 C 0.6873(4) 1.0788(3) 0.8557(3) 0.0584(9) Uani 1 1 d . . .
H24 H 0.6588 1.1086 0.7921 0.070 Uiso 1 1 calc R . .
C25 C 0.6751(4) 1.1218(4) 0.9551(3) 0.0577(9) Uani 1 1 d . . .
C26 C 0.7191(5) 1.0775(4) 1.0479(3) 0.0739(12) Uani 1 1 d . . .
H26 H 0.7123 1.1060 1.1160 0.089 Uiso 1 1 calc R . .
C27 C 0.7735(5) 0.9908(4) 1.0413(3) 0.0656(11) Uani 1 1 d . . .
H27 H 0.8043 0.9628 1.1052 0.079 Uiso 1 1 calc R . .
C28 C 0.5996(7) 1.2512(5) 1.0516(4) 0.0955(17) Uani 1 1 d . . .
H28A H 0.5390 1.1825 1.0806 0.143 Uiso 1 1 calc R . .
H28B H 0.5583 1.3086 1.0371 0.143 Uiso 1 1 calc R . .
H28C H 0.6868 1.2913 1.1044 0.143 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








































































C29 Cl4 1.785(10) . ?
C29 Cl3 1.789(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
Cl4' C29' 1.781(10) . ?
Cl3' C29' 1.736(10) . ?
C29' H29C 0.9700 . ?
C29' H29D 0.9700 . ?
Pd1 C19 1.981(3) . ?
Pd1 C7 1.992(3) . ?
Pd1 N1 2.070(2) . ?
Pd1 Cl1 2.4255(10) . ?
Br1 C9 1.907(4) . ?
O1 C15 1.370(4) . ?
O1 C18 1.433(5) . ?
O2 C25 1.369(4) . ?
O2 C28 1.419(5) . ?
N1 C1 1.339(4) . ?
N1 C5 1.363(4) . ?
N2 C19 1.357(4) . ?
N2 C20 1.388(4) . ?
N2 C12 1.437(4) . ?
N3 C19 1.370(4) . ?
N3 C21 1.395(4) . ?
N3 C22 1.441(4) . ?
C1 C2 1.380(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.373(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.471(5) . ?
C6 C11 1.392(5) . ?
C6 C7 1.414(4) . ?
C7 C8 1.398(4) . ?
C8 C9 1.384(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(5) . ?
C10 C11 1.379(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.387(5) . ?
C12 C17 1.388(5) . ?
C13 C14 1.376(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.400(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(5) . ?
C16 C17 1.388(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 C21 1.326(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C27 1.375(5) . ?
C22 C23 1.381(5) . ?
C23 C24 1.377(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.376(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.371(6) . ?
C26 C27 1.384(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?



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























































































































Cl4 C29 Cl3 115.9(9) . . ?
Cl4 C29 H29A 108.3 . . ?
Cl3 C29 H29A 108.3 . . ?
Cl4 C29 H29B 108.3 . . ?
Cl3 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
Cl3' C29' Cl4' 114.3(9) . . ?
Cl3' C29' H29C 108.7 . . ?
Cl4' C29' H29C 108.7 . . ?
Cl3' C29' H29D 108.7 . . ?
Cl4' C29' H29D 108.7 . . ?
H29C C29' H29D 107.6 . . ?
C19 Pd1 C7 92.78(12) . . ?
C19 Pd1 N1 174.28(11) . . ?
C7 Pd1 N1 81.77(11) . . ?
C19 Pd1 Cl1 90.02(8) . . ?
C7 Pd1 Cl1 176.21(9) . . ?
N1 Pd1 Cl1 95.50(8) . . ?
C15 O1 C18 117.7(3) . . ?
C25 O2 C28 118.4(3) . . ?
C1 N1 C5 119.3(3) . . ?
C1 N1 Pd1 126.5(2) . . ?
C5 N1 Pd1 114.2(2) . . ?
C19 N2 C20 110.6(3) . . ?
C19 N2 C12 125.1(3) . . ?
C20 N2 C12 124.3(3) . . ?
C19 N3 C21 110.1(3) . . ?
C19 N3 C22 127.0(2) . . ?
C21 N3 C22 122.9(3) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 120.3(3) . . ?
N1 C5 C6 114.0(3) . . ?
C4 C5 C6 125.6(3) . . ?
C11 C6 C7 120.8(3) . . ?
C11 C6 C5 122.6(3) . . ?
C7 C6 C5 116.6(3) . . ?
C8 C7 C6 117.5(3) . . ?
C8 C7 Pd1 129.1(2) . . ?
C6 C7 Pd1 113.3(2) . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 122.3(3) . . ?
C10 C9 Br1 117.8(3) . . ?
C8 C9 Br1 119.8(3) . . ?
C11 C10 C9 118.2(3) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
C10 C11 C6 121.0(3) . . ?
C10 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
C13 C12 C17 120.0(3) . . ?
C13 C12 N2 120.7(3) . . ?
C17 C12 N2 119.3(3) . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
O1 C15 C16 125.1(3) . . ?
O1 C15 C14 115.0(3) . . ?
C16 C15 C14 119.8(3) . . ?
C15 C16 C17 119.9(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C12 C17 C16 120.1(3) . . ?
C12 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 N3 104.5(2) . . ?
N2 C19 Pd1 124.3(2) . . ?
N3 C19 Pd1 131.2(2) . . ?
C21 C20 N2 107.5(3) . . ?
C21 C20 H20 126.2 . . ?
N2 C20 H20 126.2 . . ?
C20 C21 N3 107.2(3) . . ?
C20 C21 H21 126.4 . . ?
N3 C21 H21 126.4 . . ?
C27 C22 C23 118.3(3) . . ?
C27 C22 N3 119.6(3) . . ?
C23 C22 N3 122.1(3) . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 121.2(3) . . ?
C25 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
O2 C25 C26 125.5(3) . . ?
O2 C25 C24 116.0(3) . . ?
C26 C25 C24 118.4(4) . . ?
C25 C26 C27 120.6(4) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C22 C27 C26 120.9(3) . . ?
C22 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
O2 C28 H28A 109.5 . . ?
O2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?



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



























































































C19 Pd1 N1 C1 -160.8(10) . . . . ?
C7 Pd1 N1 C1 -178.8(3) . . . . ?
Cl1 Pd1 N1 C1 3.9(3) . . . . ?
C19 Pd1 N1 C5 18.9(12) . . . . ?
C7 Pd1 N1 C5 1.0(2) . . . . ?
Cl1 Pd1 N1 C5 -176.4(2) . . . . ?
C5 N1 C1 C2 1.0(5) . . . . ?
Pd1 N1 C1 C2 -179.3(3) . . . . ?
N1 C1 C2 C3 -0.4(6) . . . . ?
C1 C2 C3 C4 -0.2(6) . . . . ?
C2 C3 C4 C5 0.2(6) . . . . ?
C1 N1 C5 C4 -1.0(4) . . . . ?
Pd1 N1 C5 C4 179.3(2) . . . . ?
C1 N1 C5 C6 179.7(3) . . . . ?
Pd1 N1 C5 C6 -0.1(3) . . . . ?
C3 C4 C5 N1 0.4(5) . . . . ?
C3 C4 C5 C6 179.7(3) . . . . ?
N1 C5 C6 C11 178.8(3) . . . . ?
C4 C5 C6 C11 -0.5(5) . . . . ?
N1 C5 C6 C7 -1.3(4) . . . . ?
C4 C5 C6 C7 179.3(3) . . . . ?
C11 C6 C7 C8 0.0(4) . . . . ?
C5 C6 C7 C8 -179.9(3) . . . . ?
C11 C6 C7 Pd1 -178.0(3) . . . . ?
C5 C6 C7 Pd1 2.2(3) . . . . ?
C19 Pd1 C7 C8 2.4(3) . . . . ?
N1 Pd1 C7 C8 -179.4(3) . . . . ?
Cl1 Pd1 C7 C8 -135.3(12) . . . . ?
C19 Pd1 C7 C6 -179.9(2) . . . . ?
N1 Pd1 C7 C6 -1.7(2) . . . . ?
Cl1 Pd1 C7 C6 42.4(14) . . . . ?
C6 C7 C8 C9 -0.5(4) . . . . ?
Pd1 C7 C8 C9 177.1(2) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C7 C8 C9 Br1 178.6(2) . . . . ?
C8 C9 C10 C11 0.7(6) . . . . ?
Br1 C9 C10 C11 -177.7(3) . . . . ?
C9 C10 C11 C6 -1.2(6) . . . . ?
C7 C6 C11 C10 0.9(5) . . . . ?
C5 C6 C11 C10 -179.3(3) . . . . ?
C19 N2 C12 C13 51.8(4) . . . . ?
C20 N2 C12 C13 -129.5(3) . . . . ?
C19 N2 C12 C17 -128.7(3) . . . . ?
C20 N2 C12 C17 50.0(4) . . . . ?
C17 C12 C13 C14 1.0(5) . . . . ?
N2 C12 C13 C14 -179.5(3) . . . . ?
C12 C13 C14 C15 -1.2(5) . . . . ?
C18 O1 C15 C16 -11.3(5) . . . . ?
C18 O1 C15 C14 169.9(4) . . . . ?
C13 C14 C15 O1 179.0(3) . . . . ?
C13 C14 C15 C16 0.2(5) . . . . ?
O1 C15 C16 C17 -177.7(3) . . . . ?
C14 C15 C16 C17 0.9(5) . . . . ?
C13 C12 C17 C16 0.2(5) . . . . ?
N2 C12 C17 C16 -179.3(3) . . . . ?
C15 C16 C17 C12 -1.2(5) . . . . ?
C20 N2 C19 N3 -0.4(3) . . . . ?
C12 N2 C19 N3 178.5(3) . . . . ?
C20 N2 C19 Pd1 177.9(2) . . . . ?
C12 N2 C19 Pd1 -3.3(4) . . . . ?
C21 N3 C19 N2 0.6(3) . . . . ?
C22 N3 C19 N2 -176.6(3) . . . . ?
C21 N3 C19 Pd1 -177.5(2) . . . . ?
C22 N3 C19 Pd1 5.3(4) . . . . ?
C7 Pd1 C19 N2 87.7(3) . . . . ?
N1 Pd1 C19 N2 70.0(12) . . . . ?
Cl1 Pd1 C19 N2 -94.9(2) . . . . ?
C7 Pd1 C19 N3 -94.5(3) . . . . ?
N1 Pd1 C19 N3 -112.3(11) . . . . ?
Cl1 Pd1 C19 N3 82.9(3) . . . . ?
C19 N2 C20 C21 -0.1(4) . . . . ?
C12 N2 C20 C21 -178.9(3) . . . . ?
N2 C20 C21 N3 0.5(4) . . . . ?
C19 N3 C21 C20 -0.7(4) . . . . ?
C22 N3 C21 C20 176.7(3) . . . . ?
C19 N3 C22 C27 168.3(3) . . . . ?
C21 N3 C22 C27 -8.6(5) . . . . ?
C19 N3 C22 C23 -14.0(5) . . . . ?
C21 N3 C22 C23 169.1(3) . . . . ?
C27 C22 C23 C24 -2.3(6) . . . . ?
N3 C22 C23 C24 180.0(3) . . . . ?
C22 C23 C24 C25 0.7(6) . . . . ?
C28 O2 C25 C26 -4.5(7) . . . . ?
C28 O2 C25 C24 176.7(4) . . . . ?
C23 C24 C25 O2 179.5(4) . . . . ?
C23 C24 C25 C26 0.7(7) . . . . ?
O2 C25 C26 C27 -179.2(4) . . . . ?
C24 C25 C26 C27 -0.5(7) . . . . ?
C23 C22 C27 C26 2.5(6) . . . . ?
N3 C22 C27 C26 -179.7(4) . . . . ?
C25 C26 C27 C22 -1.1(7) . . . . ?



_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.993

_refine_diff_density_max         0.816

_refine_diff_density_min         -0.843

_refine_diff_density_rms         0.065

_database_code_depnum_ccdc_archive 'CCDC 981474'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_201309144
_audit_creation_date             2013-09-13
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H31 Br Cl N3 Pd'
_chemical_formula_sum            'C32 H31 Br Cl N3 Pd'
_chemical_formula_weight         679.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N4O4Pd1
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'
Br Br -0.6763 1.2805 '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'
N N 0.0311 0.0180 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.7297(3)
_cell_length_b                   11.47367(16)
_cell_length_c                   27.2057(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.1390(12)
_cell_angle_gamma                90.00
_cell_volume                     5842.37(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5234
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.1820
_cell_measurement_theta_min      3.9390
_exptl_absorpt_coefficient_mu    7.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10895
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.25
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    2.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -93.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   15.0000 -180.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega  -63.00  -32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
  4 omega  -78.00  -23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000  -30.0000 55

#__ type_ start__ end____ width___ exp.time_
  5 omega -119.00  -63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -30.0000 56

#__ type_ start__ end____ width___ exp.time_
  6 omega -109.00  -83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 78

#__ type_ start__ end____ width___ exp.time_
  8 omega   44.00   96.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 52

#__ type_ start__ end____ width___ exp.time_
  9 omega  122.00  174.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
 10 omega   41.00   88.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 47

#__ type_ start__ end____ width___ exp.time_
 11 omega   42.00  102.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 12 omega   59.00   86.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 13 omega   56.00   88.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
 14 omega   41.00   71.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 30

#__ type_ start__ end____ width___ exp.time_
 15 omega   60.00   90.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 30

#__ type_ start__ end____ width___ exp.time_
 16 omega   45.00   88.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  150.0000 43

#__ type_ start__ end____ width___ exp.time_
 17 omega   46.00  103.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 57

#__ type_ start__ end____ width___ exp.time_
 18 omega   88.00  173.00   1.0000    2.9300
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 19 omega  -77.00  -32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 45

#__ type_ start__ end____ width___ exp.time_
 20 omega  -47.00    6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   30.0000  -60.0000 53
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0756759000
_diffrn_orient_matrix_UB_12      0.0475591000
_diffrn_orient_matrix_UB_13      -0.0077267000
_diffrn_orient_matrix_UB_21      -0.0252603000
_diffrn_orient_matrix_UB_22      0.1232925000
_diffrn_orient_matrix_UB_23      0.0135581000
_diffrn_orient_matrix_UB_31      0.0202155000
_diffrn_orient_matrix_UB_32      -0.0239950000
_diffrn_orient_matrix_UB_33      0.0544635000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4570
_reflns_number_total             5227
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0504P)²+7.0237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1007
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C11(H11), C14(H14),
 C16(H16), C22(H22), C23(H23), C26(H26), C28(H28)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Pd1 Pd 0.688674(14) 0.39061(2) 0.610073(9) 0.04021(10) Uani 1 1 d . . .
Br1 Br 0.54942(4) 0.80526(6) 0.52466(2) 0.0894(2) Uani 1 1 d . . .
Cl1 Cl 0.76573(7) 0.27267(9) 0.66248(4) 0.0641(3) Uani 1 1 d . . .
N1 N 0.67915(19) 0.2622(3) 0.55610(13) 0.0550(9) Uani 1 1 d . . .
N2 N 0.74504(17) 0.5761(3) 0.68037(10) 0.0413(7) Uani 1 1 d . . .
N3 N 0.63303(16) 0.5500(2) 0.68867(10) 0.0391(6) Uani 1 1 d . . .
C1 C 0.7011(3) 0.1515(4) 0.5615(2) 0.0692(13) Uani 1 1 d . . .
H1 H 0.7219 0.1276 0.5914 0.083 Uiso 1 1 calc R . .
C2 C 0.6931(3) 0.0716(5) 0.5230(3) 0.090(2) Uani 1 1 d . . .
H2 H 0.7070 -0.0057 0.5273 0.108 Uiso 1 1 calc R . .
C3 C 0.6644(3) 0.1094(6) 0.4785(3) 0.099(2) Uani 1 1 d . . .
H3 H 0.6606 0.0585 0.4520 0.119 Uiso 1 1 calc R . .
C4 C 0.6416(3) 0.2221(5) 0.47351(19) 0.0817(17) Uani 1 1 d . . .
H4 H 0.6218 0.2479 0.4436 0.098 Uiso 1 1 calc R . .
C5 C 0.6483(2) 0.2986(4) 0.51342(16) 0.0581(12) Uani 1 1 d . . .
C6 C 0.6241(2) 0.4202(4) 0.51410(14) 0.0553(11) Uani 1 1 d . . .
C7 C 0.6334(2) 0.4798(3) 0.55901(12) 0.0437(8) Uani 1 1 d . . .
C8 C 0.6100(2) 0.5946(4) 0.56109(13) 0.0485(9) Uani 1 1 d . . .
H8 H 0.6149 0.6363 0.5903 0.058 Uiso 1 1 calc R . .
C9 C 0.5790(2) 0.6472(4) 0.51931(15) 0.0570(11) Uani 1 1 d . . .
C10 C 0.5698(3) 0.5878(6) 0.47515(16) 0.0746(15) Uani 1 1 d . . .
H10 H 0.5490 0.6239 0.4476 0.089 Uiso 1 1 calc R . .
C11 C 0.5920(3) 0.4755(5) 0.47339(16) 0.0695(14) Uani 1 1 d . . .
H11 H 0.5857 0.4341 0.4441 0.083 Uiso 1 1 calc R . .
C12 C 0.8181(2) 0.5713(3) 0.66493(13) 0.0425(8) Uani 1 1 d . . .
C13 C 0.8351(2) 0.6222(3) 0.62021(14) 0.0459(9) Uani 1 1 d . . .
C14 C 0.9056(3) 0.6172(4) 0.60728(16) 0.0587(11) Uani 1 1 d . . .
H14 H 0.9180 0.6493 0.5774 0.070 Uiso 1 1 calc R . .
C15 C 0.9587(2) 0.5665(4) 0.63692(18) 0.0601(11) Uani 1 1 d . . .
C16 C 0.9393(2) 0.5220(4) 0.68150(18) 0.0624(12) Uani 1 1 d . . .
H16 H 0.9747 0.4904 0.7024 0.075 Uiso 1 1 calc R . .
C17 C 0.8698(2) 0.5224(3) 0.69640(15) 0.0518(9) Uani 1 1 d . . .
C18 C 0.7805(2) 0.6803(4) 0.58686(15) 0.0586(11) Uani 1 1 d . . .
H18A H 0.7462 0.7197 0.6062 0.088 Uiso 1 1 calc R . .
H18B H 0.7567 0.6228 0.5666 0.088 Uiso 1 1 calc R . .
H18C H 0.8037 0.7358 0.5664 0.088 Uiso 1 1 calc R . .
C19 C 1.0353(3) 0.5637(6) 0.6206(3) 0.0923(19) Uani 1 1 d . . .
H19A H 1.0475 0.6382 0.6072 0.139 Uiso 1 1 calc R . .
H19B H 1.0401 0.5047 0.5959 0.139 Uiso 1 1 calc R . .
H19C H 1.0668 0.5465 0.6483 0.139 Uiso 1 1 calc R . .
C20 C 0.8518(3) 0.4703(5) 0.74555(18) 0.0727(14) Uani 1 1 d . . .
H20A H 0.8067 0.4306 0.7424 0.109 Uiso 1 1 calc R . .
H20B H 0.8489 0.5313 0.7696 0.109 Uiso 1 1 calc R . .
H20C H 0.8884 0.4160 0.7558 0.109 Uiso 1 1 calc R . .
C21 C 0.68850(19) 0.5167(3) 0.66081(11) 0.0365(7) Uani 1 1 d . . .
C22 C 0.7260(2) 0.6432(3) 0.72016(14) 0.0490(9) Uani 1 1 d . . .
H22 H 0.7561 0.6902 0.7396 0.059 Uiso 1 1 calc R . .
C23 C 0.6564(2) 0.6273(3) 0.72518(13) 0.0493(9) Uani 1 1 d . . .
H23 H 0.6285 0.6616 0.7488 0.059 Uiso 1 1 calc R . .
C24 C 0.5582(2) 0.5204(3) 0.68067(12) 0.0412(8) Uani 1 1 d . . .
C25 C 0.5363(2) 0.4054(3) 0.68700(13) 0.0439(8) Uani 1 1 d . . .
C26 C 0.4636(2) 0.3814(4) 0.67851(15) 0.0532(10) Uani 1 1 d . . .
H26 H 0.4480 0.3048 0.6811 0.064 Uiso 1 1 calc R . .
C27 C 0.4141(2) 0.4670(4) 0.66634(14) 0.0541(10) Uani 1 1 d . . .
C28 C 0.4382(2) 0.5810(4) 0.66226(14) 0.0498(9) Uani 1 1 d . . .
H28 H 0.4054 0.6398 0.6548 0.060 Uiso 1 1 calc R . .
C29 C 0.5097(2) 0.6093(3) 0.66904(13) 0.0441(8) Uani 1 1 d . . .
C30 C 0.5860(2) 0.3101(4) 0.70441(16) 0.0586(11) Uani 1 1 d . . .
H30A H 0.6221 0.3421 0.7264 0.088 Uiso 1 1 calc R . .
H30B H 0.6081 0.2756 0.6767 0.088 Uiso 1 1 calc R . .
H30C H 0.5595 0.2517 0.7213 0.088 Uiso 1 1 calc R . .
C31 C 0.3356(3) 0.4396(5) 0.6583(2) 0.0766(14) Uani 1 1 d . . .
H31A H 0.3215 0.3831 0.6822 0.115 Uiso 1 1 calc R . .
H31B H 0.3273 0.4087 0.6258 0.115 Uiso 1 1 calc R . .
H31C H 0.3082 0.5095 0.6619 0.115 Uiso 1 1 calc R . .
C32 C 0.5308(3) 0.7367(4) 0.66484(17) 0.0616(11) Uani 1 1 d . . .
H32A H 0.5804 0.7421 0.6573 0.092 Uiso 1 1 calc R . .
H32B H 0.5230 0.7756 0.6954 0.092 Uiso 1 1 calc R . .
H32C H 0.5023 0.7730 0.6391 0.092 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
Pd1 Cl1 2.4069(11) . ?
Pd1 N1 2.083(3) . ?
Pd1 C7 1.985(4) . ?
Pd1 C21 2.000(3) . ?
Br1 C9 1.903(5) . ?
N1 C1 1.342(6) . ?
N1 C5 1.344(6) . ?
N2 C12 1.447(5) . ?
N2 C21 1.351(5) . ?
N2 C22 1.386(5) . ?
N3 C21 1.363(4) . ?
N3 C23 1.390(5) . ?
N3 C24 1.451(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.396(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.375(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.397(6) . ?
C5 C6 1.468(7) . ?
C6 C7 1.406(5) . ?
C6 C11 1.393(7) . ?
C7 C8 1.390(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(5) . ?
C9 C10 1.387(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.356(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(5) . ?
C12 C17 1.388(5) . ?
C13 C14 1.381(6) . ?
C13 C18 1.498(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.384(7) . ?
C15 C16 1.376(7) . ?
C15 C19 1.519(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.378(6) . ?
C17 C20 1.514(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C22 H22 0.9300 . ?
C22 C23 1.328(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.395(5) . ?
C24 C29 1.394(5) . ?
C25 C26 1.399(6) . ?
C25 C30 1.501(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.383(6) . ?
C27 C28 1.389(6) . ?
C27 C31 1.511(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.384(6) . ?
C29 C32 1.520(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 Cl1 93.08(11) . . ?
C7 Pd1 Cl1 171.80(11) . . ?
C7 Pd1 N1 80.95(15) . . ?
C7 Pd1 C21 95.48(14) . . ?
C21 Pd1 Cl1 90.82(10) . . ?
C21 Pd1 N1 174.87(14) . . ?
C1 N1 Pd1 125.1(3) . . ?
C1 N1 C5 120.6(4) . . ?
C5 N1 Pd1 114.4(3) . . ?
C21 N2 C12 127.0(3) . . ?
C21 N2 C22 111.5(3) . . ?
C22 N2 C12 121.4(3) . . ?
C21 N3 C23 110.5(3) . . ?
C21 N3 C24 127.1(3) . . ?
C23 N3 C24 122.2(3) . . ?
N1 C1 H1 119.5 . . ?
N1 C1 C2 121.1(6) . . ?
C2 C1 H1 119.5 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.7(6) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(6) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 120.0(5) . . ?
N1 C5 C6 114.0(3) . . ?
C4 C5 C6 126.0(5) . . ?
C7 C6 C5 116.5(4) . . ?
C11 C6 C5 123.2(4) . . ?
C11 C6 C7 120.4(5) . . ?
C6 C7 Pd1 113.7(3) . . ?
C8 C7 Pd1 128.1(3) . . ?
C8 C7 C6 117.9(4) . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 Br1 117.6(3) . . ?
C10 C9 Br1 120.5(4) . . ?
C10 C9 C8 121.9(5) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 C9 118.0(4) . . ?
C11 C10 H10 121.0 . . ?
C6 C11 H11 119.0 . . ?
C10 C11 C6 121.9(4) . . ?
C10 C11 H11 119.0 . . ?
C13 C12 N2 119.1(3) . . ?
C17 C12 N2 118.8(3) . . ?
C17 C12 C13 122.0(4) . . ?
C12 C13 C18 122.7(4) . . ?
C14 C13 C12 117.2(4) . . ?
C14 C13 C18 120.1(4) . . ?
C13 C14 H14 118.6 . . ?
C13 C14 C15 122.8(4) . . ?
C15 C14 H14 118.6 . . ?
C14 C15 C19 120.2(5) . . ?
C16 C15 C14 117.6(4) . . ?
C16 C15 C19 122.2(5) . . ?
C15 C16 H16 118.7 . . ?
C15 C16 C17 122.7(4) . . ?
C17 C16 H16 118.7 . . ?
C12 C17 C20 122.1(4) . . ?
C16 C17 C12 117.7(4) . . ?
C16 C17 C20 120.2(4) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 Pd1 128.0(3) . . ?
N2 C21 N3 104.0(3) . . ?
N3 C21 Pd1 127.4(3) . . ?
N2 C22 H22 126.7 . . ?
C23 C22 N2 106.6(3) . . ?
C23 C22 H22 126.7 . . ?
N3 C23 H23 126.3 . . ?
C22 C23 N3 107.3(3) . . ?
C22 C23 H23 126.3 . . ?
C25 C24 N3 119.4(3) . . ?
C29 C24 N3 118.7(3) . . ?
C29 C24 C25 121.9(4) . . ?
C24 C25 C26 117.1(4) . . ?
C24 C25 C30 123.1(4) . . ?
C26 C25 C30 119.8(4) . . ?
C25 C26 H26 118.7 . . ?
C27 C26 C25 122.6(4) . . ?
C27 C26 H26 118.7 . . ?
C26 C27 C28 118.1(4) . . ?
C26 C27 C31 121.8(4) . . ?
C28 C27 C31 120.1(4) . . ?
C27 C28 H28 119.1 . . ?
C29 C28 C27 121.7(4) . . ?
C29 C28 H28 119.1 . . ?
C24 C29 C32 123.6(4) . . ?
C28 C29 C24 118.5(4) . . ?
C28 C29 C32 117.9(4) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_database_code_depnum_ccdc_archive 'CCDC 981475'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dd



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C16 H14 Br N O2 Pd'

_chemical_formula_weight         438.59



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source












C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'



_symmetry_cell_setting           Triclinic

_symmetry_space_group_name_H-M   P-1



loop_

_symmetry_equiv_pos_as_xyz


'x, y, z'
'-x, -y, -z'



_cell_length_a                   11.276(2)

_cell_length_b                   12.149(2)

_cell_length_c                   12.740(3)

_cell_angle_alpha                89.520(2)

_cell_angle_beta                 76.362(2)

_cell_angle_gamma                70.109(2)

_cell_volume                     1589.9(5)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    3576

_cell_measurement_theta_min      2.34

_cell_measurement_theta_max      24.37



_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.28

_exptl_crystal_size_min          0.13

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.832

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             856

_exptl_absorpt_coefficient_mu    3.683

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.3589

_exptl_absorpt_correction_T_max  0.6460

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            11350

_diffrn_reflns_av_R_equivalents  0.0195

_diffrn_reflns_av_sigmaI/netI    0.0341

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       13

_diffrn_reflns_limit_k_min       -14

_diffrn_reflns_limit_k_max       14

_diffrn_reflns_limit_l_min       -15

_diffrn_reflns_limit_l_max       15

_diffrn_reflns_theta_min         2.24

_diffrn_reflns_theta_max         25.50

_reflns_number_total             5740

_reflns_number_gt                4086

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0770P)²+6.0339P] 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         5740

_refine_ls_number_parameters     382

_refine_ls_number_restraints     40

_refine_ls_R_factor_all          0.0812

_refine_ls_R_factor_gt           0.0545

_refine_ls_wR_factor_ref         0.1603

_refine_ls_wR_factor_gt          0.1407

_refine_ls_goodness_of_fit_ref   1.025

_refine_ls_restrained_S_all      1.034

_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_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group









































































Pd1 Pd 0.45764(6) 0.62462(4) 0.08459(4) 0.0487(2) Uani 1 1 d . . .
Pd2 Pd 0.52449(8) 0.11090(5) 0.42429(5) 0.0634(2) Uani 1 1 d . . .
Br1 Br 0.98958(12) 0.35925(13) 0.10289(12) 0.1115(4) Uani 1 1 d . . .
Br2 Br 0.03415(15) 0.09656(18) 0.36985(16) 0.1450(6) Uani 1 1 d . . .
O1 O 0.5841(5) 0.6982(4) 0.0045(4) 0.0576(13) Uani 1 1 d . . .
O2 O 0.2991(6) 0.7570(4) 0.0508(4) 0.0633(14) Uani 1 1 d . . .
O3 O 0.6531(8) 0.1760(5) 0.4716(5) 0.087(2) Uani 1 1 d . . .
O4 O 0.3688(7) 0.2450(5) 0.5072(5) 0.085(2) Uani 1 1 d . . .
N1 N 0.3455(7) 0.5423(5) 0.1723(5) 0.0536(15) Uani 1 1 d . . .
N2 N 0.6682(8) -0.0268(5) 0.3307(5) 0.0640(19) Uani 1 1 d . . .
C1 C 0.5938(8) 0.4986(6) 0.1298(6) 0.0505(18) Uani 1 1 d . . .
C2 C 0.5483(9) 0.4230(6) 0.1986(6) 0.056(2) Uani 1 1 d . . .
C3 C 0.6330(10) 0.3311(7) 0.2393(7) 0.068(2) Uani 1 1 d . . .
H3 H 0.6012 0.2826 0.2859 0.081 Uiso 1 1 calc R . .
C4 C 0.7620(10) 0.3125(8) 0.2110(8) 0.074(3) Uani 1 1 d . . .
H4 H 0.8198 0.2503 0.2368 0.089 Uiso 1 1 calc R . .
C5 C 0.8067(9) 0.3865(8) 0.1436(7) 0.069(2) Uani 1 1 d . . .
C6 C 0.7238(9) 0.4800(7) 0.1021(6) 0.062(2) Uani 1 1 d . . .
H6 H 0.7566 0.5286 0.0565 0.075 Uiso 1 1 calc R . .
C7 C 0.4080(8) 0.4474(6) 0.2214(6) 0.0526(19) Uani 1 1 d . . .
C8 C 0.3373(11) 0.3865(8) 0.2840(7) 0.072(3) Uani 1 1 d . . .
H8 H 0.3796 0.3215 0.3173 0.087 Uiso 1 1 calc R . .
C9 C 0.2069(12) 0.4210(10) 0.2971(9) 0.088(3) Uani 1 1 d . . .
H9 H 0.1598 0.3802 0.3400 0.106 Uiso 1 1 calc R . .
C10 C 0.1443(11) 0.5156(9) 0.2475(9) 0.089(3) Uani 1 1 d . . .
H10 H 0.0547 0.5398 0.2561 0.106 Uiso 1 1 calc R . .
C11 C 0.2164(10) 0.5747(8) 0.1843(7) 0.071(2) Uani 1 1 d . . .
H11 H 0.1747 0.6384 0.1493 0.085 Uiso 1 1 calc R . .
C12 C 0.6610(10) 0.8333(8) -0.0927(8) 0.077(3) Uani 1 1 d . . .
H12A H 0.7102 0.8331 -0.0406 0.115 Uiso 1 1 calc R . .
H12B H 0.6272 0.9114 -0.1144 0.115 Uiso 1 1 calc R . .
H12C H 0.7163 0.7815 -0.1550 0.115 Uiso 1 1 calc R . .
C13 C 0.5523(9) 0.7931(6) -0.0438(6) 0.057(2) Uani 1 1 d . . .
C14 C 0.4300(10) 0.8575(7) -0.0530(7) 0.070(2) Uani 1 1 d . . .
H14 H 0.4241 0.9202 -0.0963 0.084 Uiso 1 1 calc R . .
C15 C 0.3118(10) 0.8410(7) -0.0053(7) 0.065(2) Uani 1 1 d . . .
C16 C 0.1848(11) 0.9286(8) -0.0181(9) 0.092(3) Uani 1 1 d . . .
H16A H 0.1141 0.9046 0.0191 0.137 Uiso 0.50 1 calc PR . .
H16B H 0.1860 0.9320 -0.0937 0.137 Uiso 0.50 1 calc PR . .
H16C H 0.1735 1.0047 0.0120 0.137 Uiso 0.50 1 calc PR . .
H16D H 0.2016 0.9896 -0.0608 0.137 Uiso 0.50 1 calc PR . .
H16E H 0.1297 0.9622 0.0519 0.137 Uiso 0.50 1 calc PR . .
H16F H 0.1422 0.8896 -0.0538 0.137 Uiso 0.50 1 calc PR . .
C17 C 0.4883(10) -0.0566(7) 0.2945(6) 0.066(2) Uani 1 1 d . . .
C18 C 0.4131(10) 0.0464(7) 0.3675(6) 0.065(2) Uani 1 1 d . . .
C19 C 0.2815(10) 0.0861(8) 0.3882(6) 0.070(2) Uani 1 1 d D . .
H19 H 0.2338 0.1521 0.4361 0.084 Uiso 1 1 calc R . .
C20 C 0.2170(11) 0.0327(10) 0.3413(9) 0.085(3) Uani 1 1 d . . .
C21 C 0.2841(13) -0.0660(10) 0.2724(8) 0.084(3) Uani 1 1 d D . .
H21 H 0.2387 -0.1024 0.2415 0.100 Uiso 1 1 calc R . .
C22 C 0.4126(13) -0.1102(9) 0.2492(7) 0.078(3) Uani 1 1 d . . .
H22 H 0.4558 -0.1777 0.2023 0.094 Uiso 1 1 calc R . .
C23 C 0.6247(9) -0.0947(7) 0.2751(6) 0.062(2) Uani 1 1 d U . .
C24 C 0.7155(11) -0.1884(8) 0.2060(7) 0.077(2) Uani 1 1 d U . .
H24 H 0.6880 -0.2340 0.1657 0.093 Uiso 1 1 calc R . .
C25 C 0.8476(11) -0.2145(9) 0.1968(9) 0.097(3) Uani 1 1 d DU . .
H25 H 0.9060 -0.2801 0.1524 0.117 Uiso 1 1 calc R . .
C26 C 0.8982(11) -0.1469(8) 0.2512(8) 0.105(3) Uani 1 1 d DU . .
H26 H 0.9864 -0.1607 0.2423 0.126 Uiso 1 1 calc R . .
C27 C 0.7965(10) -0.0550(8) 0.3211(7) 0.084(3) Uani 1 1 d DU . .
H27 H 0.8211 -0.0099 0.3645 0.100 Uiso 1 1 calc R . .
C28 C 0.7280(16) 0.3025(12) 0.5539(10) 0.137(6) Uani 1 1 d . . .
H28A H 0.7817 0.2371 0.5840 0.206 Uiso 1 1 calc R . .
H28B H 0.6929 0.3699 0.6053 0.206 Uiso 1 1 calc R . .
H28C H 0.7793 0.3196 0.4887 0.206 Uiso 1 1 calc R . .
C29 C 0.6182(16) 0.2725(11) 0.5284(8) 0.099(4) Uani 1 1 d . . .
C30 C 0.4902(18) 0.3465(10) 0.5692(8) 0.105(5) Uani 1 1 d . . .
H30 H 0.4790 0.4144 0.6095 0.126 Uiso 1 1 calc R . .
C31 C 0.3773(16) 0.3319(8) 0.5575(7) 0.099(4) Uani 1 1 d . . .
C32 C 0.2443(14) 0.4243(10) 0.6071(9) 0.123(5) Uani 1 1 d . . .
H32A H 0.2116 0.4691 0.5511 0.185 Uiso 1 1 calc R . .
H32B H 0.2526 0.4757 0.6596 0.185 Uiso 1 1 calc R . .
H32C H 0.1851 0.3863 0.6418 0.185 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















































































Pd1 C1 1.958(7) . ?
Pd1 N1 2.006(6) . ?
Pd1 O1 2.010(5) . ?
Pd1 O2 2.088(5) . ?
Pd2 C18 1.955(9) . ?
Pd2 O4 2.015(7) . ?
Pd2 N2 2.031(7) . ?
Pd2 O3 2.072(7) . ?
Br1 C5 1.914(9) . ?
Br2 C20 1.884(11) . ?
O1 C13 1.284(8) . ?
O2 C15 1.269(9) . ?
O3 C29 1.272(12) . ?
O4 C31 1.282(12) . ?
N1 C11 1.342(11) . ?
N1 C7 1.364(9) . ?
N2 C27 1.343(11) . ?
N2 C23 1.369(10) . ?
C1 C6 1.363(11) . ?
C1 C2 1.404(10) . ?
C2 C3 1.389(11) . ?
C2 C7 1.463(12) . ?
C3 C4 1.351(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.382(11) . ?
C8 C9 1.354(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(13) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.473(12) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.367(12) . ?
C14 C15 1.409(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.510(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16D 0.9600 . ?
C16 H16E 0.9600 . ?
C16 H16F 0.9600 . ?
C17 C23 1.407(13) . ?
C17 C18 1.441(11) . ?
C17 C22 1.449(13) . ?
C18 C19 1.355(13) . ?
C19 C20 1.356(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.367(15) . ?
C21 C22 1.322(14) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.384(12) . ?
C24 C25 1.389(14) . ?
C24 H24 0.9300 . ?
C25 C26 1.412(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.421(8) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.507(17) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.390(18) . ?
C30 C31 1.385(18) . ?
C30 H30 0.9300 . ?
C31 C32 1.525(17) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?



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 Pd1 N1 81.5(3) . . ?
C1 Pd1 O1 92.9(3) . . ?
N1 Pd1 O1 174.1(2) . . ?
C1 Pd1 O2 174.1(3) . . ?
N1 Pd1 O2 93.2(2) . . ?
O1 Pd1 O2 92.3(2) . . ?
C18 Pd2 O4 91.3(3) . . ?
C18 Pd2 N2 82.5(4) . . ?
O4 Pd2 N2 173.6(3) . . ?
C18 Pd2 O3 175.2(3) . . ?
O4 Pd2 O3 92.2(3) . . ?
N2 Pd2 O3 93.7(3) . . ?
C13 O1 Pd1 124.5(6) . . ?
C15 O2 Pd1 122.5(6) . . ?
C29 O3 Pd2 123.8(9) . . ?
C31 O4 Pd2 123.5(9) . . ?
C11 N1 C7 119.7(7) . . ?
C11 N1 Pd1 124.3(5) . . ?
C7 N1 Pd1 116.0(6) . . ?
C27 N2 C23 119.8(8) . . ?
C27 N2 Pd2 126.0(6) . . ?
C23 N2 Pd2 114.2(6) . . ?
C6 C1 C2 118.9(7) . . ?
C6 C1 Pd1 126.5(6) . . ?
C2 C1 Pd1 114.6(6) . . ?
C3 C2 C1 121.2(8) . . ?
C3 C2 C7 123.6(8) . . ?
C1 C2 C7 115.2(7) . . ?
C4 C3 C2 119.6(8) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.2(8) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 122.4(9) . . ?
C4 C5 Br1 119.1(7) . . ?
C6 C5 Br1 118.5(7) . . ?
C1 C6 C5 118.6(8) . . ?
C1 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N1 C7 C8 119.5(8) . . ?
N1 C7 C2 112.7(7) . . ?
C8 C7 C2 127.8(7) . . ?
C9 C8 C7 120.4(9) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.1(9) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 118.8(10) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N1 C11 C10 121.5(9) . . ?
N1 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 C14 126.3(8) . . ?
O1 C13 C12 114.8(8) . . ?
C14 C13 C12 118.9(7) . . ?
C13 C14 C15 128.2(8) . . ?
C13 C14 H14 115.9 . . ?
C15 C14 H14 115.9 . . ?
O2 C15 C14 126.0(8) . . ?
O2 C15 C16 114.0(9) . . ?
C14 C15 C16 120.0(8) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C16 H16D 109.5 . . ?
H16A C16 H16D 141.1 . . ?
H16B C16 H16D 56.3 . . ?
H16C C16 H16D 56.3 . . ?
C15 C16 H16E 109.5 . . ?
H16A C16 H16E 56.3 . . ?
H16B C16 H16E 141.1 . . ?
H16C C16 H16E 56.3 . . ?
H16D C16 H16E 109.5 . . ?
C15 C16 H16F 109.5 . . ?
H16A C16 H16F 56.3 . . ?
H16B C16 H16F 56.3 . . ?
H16C C16 H16F 141.1 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
C23 C17 C18 117.8(8) . . ?
C23 C17 C22 127.1(8) . . ?
C18 C17 C22 115.2(10) . . ?
C19 C18 C17 119.6(8) . . ?
C19 C18 Pd2 128.7(7) . . ?
C17 C18 Pd2 111.7(7) . . ?
C18 C19 C20 122.1(9) . . ?
C18 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C19 C20 C21 120.4(11) . . ?
C19 C20 Br2 119.7(9) . . ?
C21 C20 Br2 119.9(9) . . ?
C22 C21 C20 120.8(10) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C17 122.0(9) . . ?
C21 C22 H22 119.0 . . ?
C17 C22 H22 119.0 . . ?
N2 C23 C24 118.6(9) . . ?
N2 C23 C17 113.8(7) . . ?
C24 C23 C17 127.7(9) . . ?
C23 C24 C25 120.2(9) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 123.7(10) . . ?
C24 C25 H25 118.2 . . ?
C26 C25 H25 118.2 . . ?
C25 C26 C27 111.0(10) . . ?
C25 C26 H26 124.5 . . ?
C27 C26 H26 124.5 . . ?
N2 C27 C26 126.4(9) . . ?
N2 C27 H27 116.8 . . ?
C26 C27 H27 116.8 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 C29 C30 125.1(12) . . ?
O3 C29 C28 114.9(14) . . ?
C30 C29 C28 119.9(11) . . ?
C31 C30 C29 128.2(10) . . ?
C31 C30 H30 115.9 . . ?
C29 C30 H30 115.9 . . ?
O4 C31 C30 126.9(12) . . ?
O4 C31 C32 112.4(13) . . ?
C30 C31 C32 120.7(11) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?



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












































































































C1 Pd1 O1 C13 -177.7(6) . . . . ?
N1 Pd1 O1 C13 -160.5(19) . . . . ?
O2 Pd1 O1 C13 -0.5(6) . . . . ?
C1 Pd1 O2 C15 153(2) . . . . ?
N1 Pd1 O2 C15 179.3(6) . . . . ?
O1 Pd1 O2 C15 1.3(6) . . . . ?
C18 Pd2 O3 C29 135(3) . . . . ?
O4 Pd2 O3 C29 -3.1(7) . . . . ?
N2 Pd2 O3 C29 174.6(7) . . . . ?
C18 Pd2 O4 C31 -172.8(7) . . . . ?
N2 Pd2 O4 C31 -155(2) . . . . ?
O3 Pd2 O4 C31 4.0(6) . . . . ?
C1 Pd1 N1 C11 -178.1(7) . . . . ?
O1 Pd1 N1 C11 164.5(19) . . . . ?
O2 Pd1 N1 C11 4.5(6) . . . . ?
C1 Pd1 N1 C7 1.7(5) . . . . ?
O1 Pd1 N1 C7 -16(2) . . . . ?
O2 Pd1 N1 C7 -175.7(5) . . . . ?
C18 Pd2 N2 C27 -178.7(7) . . . . ?
O4 Pd2 N2 C27 163(2) . . . . ?
O3 Pd2 N2 C27 4.4(7) . . . . ?
C18 Pd2 N2 C23 0.5(5) . . . . ?
O4 Pd2 N2 C23 -18(2) . . . . ?
O3 Pd2 N2 C23 -176.4(5) . . . . ?
N1 Pd1 C1 C6 178.6(7) . . . . ?
O1 Pd1 C1 C6 -3.1(7) . . . . ?
O2 Pd1 C1 C6 -155(2) . . . . ?
N1 Pd1 C1 C2 -2.3(5) . . . . ?
O1 Pd1 C1 C2 175.9(5) . . . . ?
O2 Pd1 C1 C2 24(3) . . . . ?
C6 C1 C2 C3 0.6(11) . . . . ?
Pd1 C1 C2 C3 -178.5(6) . . . . ?
C6 C1 C2 C7 -178.3(6) . . . . ?
Pd1 C1 C2 C7 2.6(8) . . . . ?
C1 C2 C3 C4 -1.1(12) . . . . ?
C7 C2 C3 C4 177.7(8) . . . . ?
C2 C3 C4 C5 1.1(13) . . . . ?
C3 C4 C5 C6 -0.7(13) . . . . ?
C3 C4 C5 Br1 -179.6(7) . . . . ?
C2 C1 C6 C5 -0.2(11) . . . . ?
Pd1 C1 C6 C5 178.9(6) . . . . ?
C4 C5 C6 C1 0.2(12) . . . . ?
Br1 C5 C6 C1 179.1(6) . . . . ?
C11 N1 C7 C8 -0.7(10) . . . . ?
Pd1 N1 C7 C8 179.5(5) . . . . ?
C11 N1 C7 C2 179.0(7) . . . . ?
Pd1 N1 C7 C2 -0.8(7) . . . . ?
C3 C2 C7 N1 180.0(7) . . . . ?
C1 C2 C7 N1 -1.1(9) . . . . ?
C3 C2 C7 C8 -0.3(12) . . . . ?
C1 C2 C7 C8 178.5(7) . . . . ?
N1 C7 C8 C9 -0.4(12) . . . . ?
C2 C7 C8 C9 179.9(8) . . . . ?
C7 C8 C9 C10 0.7(15) . . . . ?
C8 C9 C10 C11 0.0(16) . . . . ?
C7 N1 C11 C10 1.4(12) . . . . ?
Pd1 N1 C11 C10 -178.8(7) . . . . ?
C9 C10 C11 N1 -1.1(15) . . . . ?
Pd1 O1 C13 C14 -2.6(10) . . . . ?
Pd1 O1 C13 C12 177.2(5) . . . . ?
O1 C13 C14 C15 5.7(14) . . . . ?
C12 C13 C14 C15 -174.1(8) . . . . ?
Pd1 O2 C15 C14 0.8(11) . . . . ?
Pd1 O2 C15 C16 -178.8(6) . . . . ?
C13 C14 C15 O2 -4.6(15) . . . . ?
C13 C14 C15 C16 174.9(9) . . . . ?
C23 C17 C18 C19 179.9(7) . . . . ?
C22 C17 C18 C19 -0.5(10) . . . . ?
C23 C17 C18 Pd2 0.1(8) . . . . ?
C22 C17 C18 Pd2 179.7(5) . . . . ?
O4 Pd2 C18 C19 -2.1(7) . . . . ?
N2 Pd2 C18 C19 179.9(7) . . . . ?
O3 Pd2 C18 C19 -140(3) . . . . ?
O4 Pd2 C18 C17 177.7(5) . . . . ?
N2 Pd2 C18 C17 -0.3(5) . . . . ?
O3 Pd2 C18 C17 40(4) . . . . ?
C17 C18 C19 C20 -0.7(12) . . . . ?
Pd2 C18 C19 C20 179.1(6) . . . . ?
C18 C19 C20 C21 1.4(14) . . . . ?
C18 C19 C20 Br2 -177.6(6) . . . . ?
C19 C20 C21 C22 -0.9(15) . . . . ?
Br2 C20 C21 C22 178.2(7) . . . . ?
C20 C21 C22 C17 -0.4(15) . . . . ?
C23 C17 C22 C21 -179.4(8) . . . . ?
C18 C17 C22 C21 1.0(12) . . . . ?
C27 N2 C23 C24 -2.9(11) . . . . ?
Pd2 N2 C23 C24 177.8(6) . . . . ?
C27 N2 C23 C17 178.7(7) . . . . ?
Pd2 N2 C23 C17 -0.6(8) . . . . ?
C18 C17 C23 N2 0.4(10) . . . . ?
C22 C17 C23 N2 -179.2(7) . . . . ?
C18 C17 C23 C24 -177.8(8) . . . . ?
C22 C17 C23 C24 2.6(13) . . . . ?
N2 C23 C24 C25 2.2(12) . . . . ?
C17 C23 C24 C25 -179.7(9) . . . . ?
C23 C24 C25 C26 -3.0(16) . . . . ?
C24 C25 C26 C27 4.0(15) . . . . ?
C23 N2 C27 C26 4.7(14) . . . . ?
Pd2 N2 C27 C26 -176.1(8) . . . . ?
C25 C26 C27 N2 -5.0(15) . . . . ?
Pd2 O3 C29 C30 1.7(13) . . . . ?
Pd2 O3 C29 C28 179.6(7) . . . . ?
O3 C29 C30 C31 0.1(18) . . . . ?
C28 C29 C30 C31 -177.8(11) . . . . ?
Pd2 O4 C31 C30 -3.8(13) . . . . ?
Pd2 O4 C31 C32 176.3(6) . . . . ?
C29 C30 C31 O4 1.1(18) . . . . ?
C29 C30 C31 C32 -179.0(10) . . . . ?



_diffrn_measured_fraction_theta_max 0.967

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.967

_refine_diff_density_max         3.754

_refine_diff_density_min         -0.958

_refine_diff_density_rms         0.118

_database_code_depnum_ccdc_archive 'CCDC 981476'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_bb



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C22.50 H15 Br2 Cl2 Ir N2'

_chemical_formula_weight         736.28



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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Tetragonal

_symmetry_space_group_name_H-M   I4(1)cd



loop_

_symmetry_equiv_pos_as_xyz
















'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'



_cell_length_a                   16.6765(14)

_cell_length_b                   16.6765(14)

_cell_length_c                   32.620(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     9071.9(19)

_cell_formula_units_Z            16

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    8629

_cell_measurement_theta_min      2.44

_cell_measurement_theta_max      25.83



_exptl_crystal_description       block

_exptl_crystal_colour            blue

_exptl_crystal_size_max          0.32

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.21

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    2.156

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             5520

_exptl_absorpt_coefficient_mu    9.659

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.1481

_exptl_absorpt_correction_T_max  0.2362

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            32512

_diffrn_reflns_av_R_equivalents  0.1112

_diffrn_reflns_av_sigmaI/netI    0.0520

_diffrn_reflns_limit_h_min       -20

_diffrn_reflns_limit_h_max       20

_diffrn_reflns_limit_k_min       -20

_diffrn_reflns_limit_k_max       20

_diffrn_reflns_limit_l_min       -39

_diffrn_reflns_limit_l_max       39

_diffrn_reflns_theta_min         2.44

_diffrn_reflns_theta_max         25.50

_reflns_number_total             4222

_reflns_number_gt                3495

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0738P)²+0.0000P] 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 H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -0.038(17)

_refine_ls_number_reflns         4222

_refine_ls_number_parameters     281

_refine_ls_number_restraints     25

_refine_ls_R_factor_all          0.0545

_refine_ls_R_factor_gt           0.0444

_refine_ls_wR_factor_ref         0.1135

_refine_ls_wR_factor_gt          0.1087

_refine_ls_goodness_of_fit_ref   1.001

_refine_ls_restrained_S_all      1.001

_refine_ls_shift/su_max          0.004

_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
















































Ir1 Ir 0.008737(16) 0.88791(2) 0.87261(3) 0.04099(10) Uani 1 1 d . . .
Br1 Br 0.13796(8) 0.65627(9) 0.75367(4) 0.0862(4) Uani 1 1 d . . .
Br2 Br -0.08354(10) 0.63918(9) 0.99166(4) 0.0960(5) Uani 1 1 d . . .
Cl1 Cl 0.0000 1.0000 0.82217(11) 0.0512(11) Uani 1 2 d S . .
Cl2 Cl 0.0000 1.0000 0.92467(11) 0.0438(10) Uani 1 2 d S . .
N1 N -0.1142(4) 0.8711(5) 0.8710(3) 0.0456(18) Uani 1 1 d . . .
N2 N 0.1332(4) 0.8904(5) 0.8745(3) 0.0497(19) Uani 1 1 d . . .
C1 C 0.0036(6) 0.8058(7) 0.8281(3) 0.050(3) Uani 1 1 d . . .
C2 C 0.0660(6) 0.7691(6) 0.8083(3) 0.051(3) Uani 1 1 d . . .
H2 H 0.1186 0.7827 0.8147 0.061 Uiso 1 1 calc R . .
C3 C 0.0506(7) 0.7116(6) 0.7784(3) 0.062(3) Uani 1 1 d . . .
C4 C -0.0281(8) 0.6896(7) 0.7674(3) 0.068(3) Uani 1 1 d . . .
H4 H -0.0373 0.6514 0.7472 0.081 Uiso 1 1 calc R . .
C5 C -0.0901(7) 0.7253(7) 0.7871(4) 0.067(3) Uani 1 1 d . . .
H5 H -0.1422 0.7121 0.7795 0.081 Uiso 1 1 calc R . .
C6 C -0.0785(6) 0.7811(6) 0.8183(3) 0.046(2) Uani 1 1 d . . .
C7 C -0.1400(6) 0.8187(6) 0.8422(3) 0.051(3) Uani 1 1 d . . .
C8 C -0.2213(6) 0.8037(7) 0.8379(4) 0.062(3) Uani 1 1 d . . .
H8 H -0.2397 0.7699 0.8172 0.075 Uiso 1 1 calc R . .
C9 C -0.2746(6) 0.8396(8) 0.8645(5) 0.076(4) Uani 1 1 d . . .
H9 H -0.3292 0.8293 0.8621 0.092 Uiso 1 1 calc R . .
C10 C -0.2486(7) 0.8888(8) 0.8938(4) 0.070(4) Uani 1 1 d . . .
H10 H -0.2843 0.9124 0.9121 0.085 Uiso 1 1 calc R . .
C11 C -0.1666(6) 0.9040(6) 0.8964(3) 0.049(2) Uani 1 1 d . . .
H11 H -0.1480 0.9385 0.9167 0.059 Uiso 1 1 calc R . .
C12 C 0.0273(7) 0.8056(6) 0.9157(3) 0.049(2) Uani 1 1 d . . .
C13 C -0.0294(7) 0.7551(7) 0.9354(3) 0.056(3) Uani 1 1 d . . .
H13 H -0.0829 0.7573 0.9275 0.067 Uiso 1 1 calc R . .
C14 C -0.0068(7) 0.7031(9) 0.9657(4) 0.074(4) Uani 1 1 d . . .
C15 C 0.0776(8) 0.6981(8) 0.9780(4) 0.078(4) Uani 1 1 d . . .
H15 H 0.0938 0.6626 0.9984 0.094 Uiso 1 1 calc R . .
C16 C 0.1306(7) 0.7454(8) 0.9593(4) 0.071(4) Uani 1 1 d . . .
H16 H 0.1840 0.7425 0.9675 0.086 Uiso 1 1 calc R . .
C17 C 0.1100(6) 0.7998(8) 0.9277(3) 0.059(3) Uani 1 1 d . . .
C18 C 0.1659(6) 0.8479(7) 0.9047(3) 0.062(3) Uani 1 1 d . . .
C19 C 0.2498(8) 0.8429(10) 0.9108(6) 0.099(5) Uani 1 1 d . . .
H19 H 0.2726 0.8127 0.9318 0.119 Uiso 1 1 calc R . .
C20 C 0.2965(7) 0.8880(9) 0.8822(6) 0.101(6) Uani 1 1 d . . .
H20 H 0.3518 0.8910 0.8856 0.121 Uiso 1 1 calc R . .
C21 C 0.2611(8) 0.9266(8) 0.8502(5) 0.078(4) Uani 1 1 d . . .
H21 H 0.2925 0.9506 0.8301 0.094 Uiso 1 1 calc R . .
C22 C 0.1792(7) 0.9300(7) 0.8477(3) 0.063(3) Uani 1 1 d . . .
H22 H 0.1552 0.9603 0.8271 0.075 Uiso 1 1 calc R . .
C23 C 0.014(4) 0.520(2) 0.9067(8) 0.2047(10) Uani 0.50 1 d PDU . .
H23A H 0.0659 0.4932 0.9056 0.246 Uiso 0.50 1 calc PR . .
H23B H 0.0085 0.5342 0.9354 0.246 Uiso 0.50 1 calc PR . .
Cl3 Cl 0.0232(10) 0.5806(9) 0.8609(6) 0.2046(11) Uani 0.50 1 d PDU . .
Cl4 Cl -0.0308(12) 0.4288(9) 0.8966(6) 0.2061(11) Uani 0.50 1 d PDU . .






_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



























































Ir1 C12 1.989(10) . ?
Ir1 C1 1.998(12) . ?
Ir1 N1 2.070(6) . ?
Ir1 N2 2.077(6) . ?
Ir1 Cl1 2.494(3) . ?
Ir1 Cl2 2.530(3) . ?
Br1 C3 1.903(11) . ?
Br2 C14 1.868(13) . ?
Cl1 Ir1 2.494(3) 10_464 ?
Cl2 Ir1 2.530(3) 10_464 ?
N1 C11 1.323(13) . ?
N1 C7 1.352(13) . ?
N2 C18 1.329(15) . ?
N2 C22 1.337(14) . ?
C1 C2 1.369(14) . ?
C1 C6 1.466(13) . ?
C2 C3 1.392(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.410(16) . ?
C4 C5 1.354(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.433(14) . ?
C7 C8 1.387(13) . ?
C8 C9 1.380(16) . ?
C8 H8 0.9300 . ?
C9 C10 1.331(18) . ?
C9 H9 0.9300 . ?
C10 C11 1.393(15) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.420(16) . ?
C12 C17 1.437(15) . ?
C13 C14 1.367(16) . ?
C13 H13 0.9300 . ?
C14 C15 1.466(16) . ?
C15 C16 1.333(18) . ?
C15 H15 0.9300 . ?
C16 C17 1.417(17) . ?
C16 H16 0.9300 . ?
C17 C18 1.440(17) . ?
C18 C19 1.416(15) . ?
C19 C20 1.43(2) . ?
C19 H19 0.9300 . ?
C20 C21 1.36(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.370(17) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C23 0.82(5) 10_454 ?
C23 Cl4 0.96(3) 10_454 ?
C23 Cl4 1.727(19) . ?
C23 Cl3 1.812(19) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
Cl3 Cl4 1.18(2) 10_454 ?
Cl4 C23 0.96(3) 10_454 ?
Cl4 Cl3 1.18(2) 10_454 ?



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












































































































C12 Ir1 C1 92.7(4) . . ?
C12 Ir1 N1 94.5(4) . . ?
C1 Ir1 N1 81.2(4) . . ?
C12 Ir1 N2 80.6(4) . . ?
C1 Ir1 N2 94.5(4) . . ?
N1 Ir1 N2 173.4(3) . . ?
C12 Ir1 Cl1 172.9(3) . . ?
C1 Ir1 Cl1 91.8(3) . . ?
N1 Ir1 Cl1 91.5(2) . . ?
N2 Ir1 Cl1 93.6(3) . . ?
C12 Ir1 Cl2 92.5(3) . . ?
C1 Ir1 Cl2 172.8(3) . . ?
N1 Ir1 Cl2 93.5(3) . . ?
N2 Ir1 Cl2 91.3(3) . . ?
Cl1 Ir1 Cl2 83.44(6) . . ?
Ir1 Cl1 Ir1 97.46(13) 10_464 . ?
Ir1 Cl2 Ir1 95.66(13) . 10_464 ?
C11 N1 C7 119.5(8) . . ?
C11 N1 Ir1 125.6(7) . . ?
C7 N1 Ir1 114.8(6) . . ?
C18 N2 C22 120.8(9) . . ?
C18 N2 Ir1 114.9(7) . . ?
C22 N2 Ir1 124.3(8) . . ?
C2 C1 C6 118.8(10) . . ?
C2 C1 Ir1 128.1(8) . . ?
C6 C1 Ir1 113.0(7) . . ?
C1 C2 C3 119.9(10) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 122.0(10) . . ?
C2 C3 Br1 119.3(8) . . ?
C4 C3 Br1 118.6(8) . . ?
C5 C4 C3 118.4(10) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 122.3(10) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C7 126.3(9) . . ?
C5 C6 C1 118.5(9) . . ?
C7 C6 C1 115.2(9) . . ?
N1 C7 C8 119.9(10) . . ?
N1 C7 C6 115.7(8) . . ?
C8 C7 C6 124.4(10) . . ?
C9 C8 C7 119.1(11) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 120.6(11) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 118.4(12) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
N1 C11 C10 122.3(11) . . ?
N1 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C13 C12 C17 118.4(10) . . ?
C13 C12 Ir1 128.8(8) . . ?
C17 C12 Ir1 112.8(8) . . ?
C14 C13 C12 121.3(11) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C15 119.9(12) . . ?
C13 C14 Br2 120.0(9) . . ?
C15 C14 Br2 120.0(9) . . ?
C16 C15 C14 118.5(11) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 123.5(11) . . ?
C15 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C16 C17 C12 118.3(11) . . ?
C16 C17 C18 125.4(10) . . ?
C12 C17 C18 116.2(10) . . ?
N2 C18 C19 122.8(13) . . ?
N2 C18 C17 114.7(8) . . ?
C19 C18 C17 122.2(13) . . ?
C18 C19 C20 114.5(15) . . ?
C18 C19 H19 122.7 . . ?
C20 C19 H19 122.7 . . ?
C21 C20 C19 120.9(11) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 119.8(12) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
N2 C22 C21 120.9(12) . . ?
N2 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C23 C23 Cl4 153(8) 10_454 10_454 ?
C23 C23 Cl4 14(4) 10_454 . ?
Cl4 C23 Cl4 148(3) 10_454 . ?
C23 C23 Cl3 120(3) 10_454 . ?
Cl4 C23 Cl3 36.2(14) 10_454 . ?
Cl4 C23 Cl3 111.7(13) . . ?
C23 C23 H23A 98.2 10_454 . ?
Cl4 C23 H23A 98.2 10_454 . ?
Cl4 C23 H23A 88.5 . . ?
Cl3 C23 H23A 98.8 . . ?
C23 C23 H23B 98.2 10_454 . ?
Cl4 C23 H23B 98.2 10_454 . ?
Cl4 C23 H23B 110.9 . . ?
Cl3 C23 H23B 131.9 . . ?
H23A C23 H23B 103.7 . . ?
Cl4 Cl3 C23 28.5(14) 10_454 . ?
C23 Cl4 Cl3 115(2) 10_454 10_454 ?
C23 Cl4 C23 12(4) 10_454 . ?
Cl3 Cl4 C23 105.0(18) 10_454 . ?



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

















































































































C12 Ir1 Cl1 Ir1 -56(2) . . . 10_464 ?
C1 Ir1 Cl1 Ir1 174.5(3) . . . 10_464 ?
N1 Ir1 Cl1 Ir1 93.3(3) . . . 10_464 ?
N2 Ir1 Cl1 Ir1 -90.9(3) . . . 10_464 ?
Cl2 Ir1 Cl1 Ir1 0.0 . . . 10_464 ?
C12 Ir1 Cl2 Ir1 174.2(3) . . . 10_464 ?
C1 Ir1 Cl2 Ir1 -50(2) . . . 10_464 ?
N1 Ir1 Cl2 Ir1 -91.1(2) . . . 10_464 ?
N2 Ir1 Cl2 Ir1 93.5(3) . . . 10_464 ?
Cl1 Ir1 Cl2 Ir1 0.0 . . . 10_464 ?
C12 Ir1 N1 C11 82.9(8) . . . . ?
C1 Ir1 N1 C11 175.0(9) . . . . ?
N2 Ir1 N1 C11 125(4) . . . . ?
Cl1 Ir1 N1 C11 -93.4(8) . . . . ?
Cl2 Ir1 N1 C11 -9.9(8) . . . . ?
C12 Ir1 N1 C7 -93.9(7) . . . . ?
C1 Ir1 N1 C7 -1.8(7) . . . . ?
N2 Ir1 N1 C7 -51(4) . . . . ?
Cl1 Ir1 N1 C7 89.8(7) . . . . ?
Cl2 Ir1 N1 C7 173.3(7) . . . . ?
C12 Ir1 N2 C18 -7.9(8) . . . . ?
C1 Ir1 N2 C18 -99.9(8) . . . . ?
N1 Ir1 N2 C18 -51(4) . . . . ?
Cl1 Ir1 N2 C18 167.9(7) . . . . ?
Cl2 Ir1 N2 C18 84.4(8) . . . . ?
C12 Ir1 N2 C22 171.1(9) . . . . ?
C1 Ir1 N2 C22 79.1(9) . . . . ?
N1 Ir1 N2 C22 128(4) . . . . ?
Cl1 Ir1 N2 C22 -13.1(8) . . . . ?
Cl2 Ir1 N2 C22 -96.6(8) . . . . ?
C12 Ir1 C1 C2 -81.2(10) . . . . ?
N1 Ir1 C1 C2 -175.3(11) . . . . ?
N2 Ir1 C1 C2 -0.4(11) . . . . ?
Cl1 Ir1 C1 C2 93.4(10) . . . . ?
Cl2 Ir1 C1 C2 142.5(19) . . . . ?
C12 Ir1 C1 C6 95.5(8) . . . . ?
N1 Ir1 C1 C6 1.3(7) . . . . ?
N2 Ir1 C1 C6 176.3(8) . . . . ?
Cl1 Ir1 C1 C6 -89.9(7) . . . . ?
Cl2 Ir1 C1 C6 -41(3) . . . . ?
C6 C1 C2 C3 2.1(16) . . . . ?
Ir1 C1 C2 C3 178.6(8) . . . . ?
C1 C2 C3 C4 0.5(17) . . . . ?
C1 C2 C3 Br1 -175.9(8) . . . . ?
C2 C3 C4 C5 -0.8(18) . . . . ?
Br1 C3 C4 C5 175.7(9) . . . . ?
C3 C4 C5 C6 -1.7(18) . . . . ?
C4 C5 C6 C7 -176.5(11) . . . . ?
C4 C5 C6 C1 4.3(16) . . . . ?
C2 C1 C6 C5 -4.4(15) . . . . ?
Ir1 C1 C6 C5 178.6(8) . . . . ?
C2 C1 C6 C7 176.3(9) . . . . ?
Ir1 C1 C6 C7 -0.7(11) . . . . ?
C11 N1 C7 C8 4.1(14) . . . . ?
Ir1 N1 C7 C8 -178.9(8) . . . . ?
C11 N1 C7 C6 -175.1(9) . . . . ?
Ir1 N1 C7 C6 1.9(11) . . . . ?
C5 C6 C7 N1 180.0(10) . . . . ?
C1 C6 C7 N1 -0.8(13) . . . . ?
C5 C6 C7 C8 0.9(16) . . . . ?
C1 C6 C7 C8 -179.9(10) . . . . ?
N1 C7 C8 C9 -3.4(16) . . . . ?
C6 C7 C8 C9 175.7(10) . . . . ?
C7 C8 C9 C10 0.8(18) . . . . ?
C8 C9 C10 C11 1.0(19) . . . . ?
C7 N1 C11 C10 -2.3(15) . . . . ?
Ir1 N1 C11 C10 -178.9(8) . . . . ?
C9 C10 C11 N1 -0.3(18) . . . . ?
C1 Ir1 C12 C13 -80.0(10) . . . . ?
N1 Ir1 C12 C13 1.4(10) . . . . ?
N2 Ir1 C12 C13 -174.1(10) . . . . ?
Cl1 Ir1 C12 C13 150.2(19) . . . . ?
Cl2 Ir1 C12 C13 95.1(9) . . . . ?
C1 Ir1 C12 C17 100.9(8) . . . . ?
N1 Ir1 C12 C17 -177.7(8) . . . . ?
N2 Ir1 C12 C17 6.8(7) . . . . ?
Cl1 Ir1 C12 C17 -29(3) . . . . ?
Cl2 Ir1 C12 C17 -84.1(7) . . . . ?
C17 C12 C13 C14 1.4(16) . . . . ?
Ir1 C12 C13 C14 -177.7(10) . . . . ?
C12 C13 C14 C15 -0.9(19) . . . . ?
C12 C13 C14 Br2 178.7(9) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
Br2 C14 C15 C16 -179.0(11) . . . . ?
C14 C15 C16 C17 -1(2) . . . . ?
C15 C16 C17 C12 1.3(19) . . . . ?
C15 C16 C17 C18 -175.4(12) . . . . ?
C13 C12 C17 C16 -1.6(15) . . . . ?
Ir1 C12 C17 C16 177.7(9) . . . . ?
C13 C12 C17 C18 175.5(9) . . . . ?
Ir1 C12 C17 C18 -5.3(12) . . . . ?
C22 N2 C18 C19 1.2(17) . . . . ?
Ir1 N2 C18 C19 -179.8(10) . . . . ?
C22 N2 C18 C17 -171.9(9) . . . . ?
Ir1 N2 C18 C17 7.1(12) . . . . ?
C16 C17 C18 N2 175.5(11) . . . . ?
C12 C17 C18 N2 -1.3(14) . . . . ?
C16 C17 C18 C19 2.3(18) . . . . ?
C12 C17 C18 C19 -174.5(11) . . . . ?
N2 C18 C19 C20 0.6(18) . . . . ?
C17 C18 C19 C20 173.2(12) . . . . ?
C18 C19 C20 C21 -5(2) . . . . ?
C19 C20 C21 C22 7(2) . . . . ?
C18 N2 C22 C21 1.1(16) . . . . ?
Ir1 N2 C22 C21 -177.8(8) . . . . ?
C20 C21 C22 N2 -5.4(18) . . . . ?
C23 C23 Cl3 Cl4 163(16) 10_454 . . 10_454 ?
Cl4 C23 Cl3 Cl4 176(8) . . . 10_454 ?
Cl4 C23 Cl4 C23 -125(35) 10_454 . . 10_454 ?
Cl3 C23 Cl4 C23 -129(26) . . . 10_454 ?
C23 C23 Cl4 Cl3 149(23) 10_454 . . 10_454 ?
Cl4 C23 Cl4 Cl3 24(11) 10_454 . . 10_454 ?
Cl3 C23 Cl4 Cl3 20(4) . . . 10_454 ?



_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         1.195

_refine_diff_density_min         -0.902

_refine_diff_density_rms         0.148

_database_code_depnum_ccdc_archive 'CCDC 981477'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C28 H23 Br2 Cl2 Ir N2 O2'

_chemical_formula_weight         842.40



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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   P2(1)/n



loop_

_symmetry_equiv_pos_as_xyz




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



_cell_length_a                   11.480(3)

_cell_length_b                   16.018(4)

_cell_length_c                   16.194(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 105.110(3)

_cell_angle_gamma                90.00

_cell_volume                     2874.8(11)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    3796

_cell_measurement_theta_min      2.33

_cell_measurement_theta_max      22.47



_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.11

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.946

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1608

_exptl_absorpt_coefficient_mu    7.638

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.1752

_exptl_absorpt_correction_T_max  0.4871

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            21258

_diffrn_reflns_av_R_equivalents  0.0741

_diffrn_reflns_av_sigmaI/netI    0.0694

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       13

_diffrn_reflns_limit_k_min       -19

_diffrn_reflns_limit_k_max       19

_diffrn_reflns_limit_l_min       -19

_diffrn_reflns_limit_l_max       19

_diffrn_reflns_theta_min         2.33

_diffrn_reflns_theta_max         25.50

_reflns_number_total             5328

_reflns_number_gt                3776

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1019P)²+12.0458P] 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         5328

_refine_ls_number_parameters     336

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0943

_refine_ls_R_factor_gt           0.0604

_refine_ls_wR_factor_ref         0.1826

_refine_ls_wR_factor_gt          0.1586

_refine_ls_goodness_of_fit_ref   1.068

_refine_ls_restrained_S_all      1.068

_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_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group




























































Ir1 Ir 0.93038(4) 0.23917(3) 0.50417(3) 0.03690(19) Uani 1 1 d . . .
Br1 Br 1.43278(15) 0.12587(12) 0.64560(13) 0.0819(6) Uani 1 1 d . . .
Br2 Br 0.8366(3) 0.28039(14) 0.84234(14) 0.1093(9) Uani 1 1 d . . .
O1 O 0.7777(8) 0.3170(5) 0.4456(6) 0.046(2) Uani 1 1 d . . .
O2 O 0.9248(8) 0.1893(5) 0.3806(5) 0.047(2) Uani 1 1 d . . .
Cl1 Cl 0.6255(8) 0.4535(6) 0.6682(6) 0.170(3) Uani 1 1 d . . .
Cl2 Cl 0.4736(10) 0.3569(10) 0.5363(6) 0.227(6) Uani 1 1 d . . .
N1 N 0.8274(9) 0.1406(6) 0.5242(6) 0.042(2) Uani 1 1 d . . .
N2 N 1.0385(10) 0.3354(6) 0.4935(7) 0.045(3) Uani 1 1 d . . .
C1 C 0.7079(13) 0.1403(9) 0.5029(9) 0.054(3) Uani 1 1 d . . .
H1 H 0.6670 0.1875 0.4771 0.065 Uiso 1 1 calc R . .
C2 C 0.6432(14) 0.0735(10) 0.5176(10) 0.067(4) Uani 1 1 d . . .
H2 H 0.5594 0.0742 0.5000 0.080 Uiso 1 1 calc R . .
C3 C 0.7047(15) 0.0036(11) 0.5596(10) 0.070(5) Uani 1 1 d . . .
H3 H 0.6625 -0.0422 0.5721 0.084 Uiso 1 1 calc R . .
C4 C 0.8285(15) 0.0041(8) 0.5818(8) 0.061(4) Uani 1 1 d . . .
H4 H 0.8714 -0.0414 0.6099 0.073 Uiso 1 1 calc R . .
C5 C 0.8890(12) 0.0733(7) 0.5621(8) 0.046(3) Uani 1 1 d . . .
C6 C 1.0207(12) 0.0831(7) 0.5814(8) 0.045(3) Uani 1 1 d . . .
C7 C 1.0614(11) 0.1598(7) 0.5591(7) 0.041(3) Uani 1 1 d . . .
C8 C 1.1860(12) 0.1705(7) 0.5778(8) 0.048(3) Uani 1 1 d . . .
H8 H 1.2176 0.2204 0.5635 0.057 Uiso 1 1 calc R . .
C9 C 1.2618(12) 0.1086(9) 0.6167(8) 0.052(3) Uani 1 1 d . . .
C10 C 1.2211(14) 0.0319(8) 0.6372(9) 0.061(4) Uani 1 1 d . . .
H10 H 1.2751 -0.0099 0.6624 0.073 Uiso 1 1 calc R . .
C11 C 1.1000(13) 0.0195(8) 0.6195(8) 0.055(4) Uani 1 1 d . . .
H11 H 1.0698 -0.0313 0.6326 0.066 Uiso 1 1 calc R . .
C12 C 1.0868(13) 0.3494(9) 0.4277(9) 0.056(4) Uani 1 1 d . . .
H12 H 1.0714 0.3112 0.3830 0.067 Uiso 1 1 calc R . .
C13 C 1.1582(14) 0.4176(10) 0.4228(11) 0.068(4) Uani 1 1 d . . .
H13 H 1.1905 0.4252 0.3763 0.082 Uiso 1 1 calc R . .
C14 C 1.1797(14) 0.4732(9) 0.4883(12) 0.070(5) Uani 1 1 d . . .
H14 H 1.2267 0.5202 0.4865 0.083 Uiso 1 1 calc R . .
C15 C 1.1341(14) 0.4613(9) 0.5552(10) 0.060(4) Uani 1 1 d . . .
H15 H 1.1499 0.5000 0.5996 0.072 Uiso 1 1 calc R . .
C16 C 1.0642(12) 0.3926(7) 0.5596(9) 0.052(4) Uani 1 1 d . . .
C17 C 1.0080(11) 0.3698(8) 0.6299(8) 0.044(3) Uani 1 1 d . . .
C18 C 0.9430(12) 0.2933(8) 0.6172(8) 0.043(3) Uani 1 1 d . . .
C19 C 0.8908(13) 0.2677(8) 0.6808(9) 0.049(3) Uani 1 1 d . . .
H19 H 0.8465 0.2184 0.6751 0.058 Uiso 1 1 calc R . .
C20 C 0.9062(15) 0.3180(10) 0.7546(9) 0.064(4) Uani 1 1 d . . .
C21 C 0.9672(17) 0.3941(10) 0.7650(10) 0.074(5) Uani 1 1 d . . .
H21 H 0.9734 0.4274 0.8130 0.089 Uiso 1 1 calc R . .
C22 C 1.0163(13) 0.4165(8) 0.7017(10) 0.061(4) Uani 1 1 d . . .
H22 H 1.0584 0.4666 0.7070 0.073 Uiso 1 1 calc R . .
C23 C 0.6200(13) 0.3753(9) 0.3415(10) 0.069(4) Uani 1 1 d . . .
H23A H 0.5576 0.3586 0.3676 0.103 Uiso 1 1 calc R . .
H23B H 0.5888 0.3751 0.2804 0.103 Uiso 1 1 calc R . .
H23C H 0.6472 0.4304 0.3603 0.103 Uiso 1 1 calc R . .
C24 C 0.7249(12) 0.3146(7) 0.3668(9) 0.049(3) Uani 1 1 d . . .
C25 C 0.7487(15) 0.2635(9) 0.3059(10) 0.064(4) Uani 1 1 d . . .
H25 H 0.6941 0.2670 0.2524 0.077 Uiso 1 1 calc R . .
C26 C 0.8416(13) 0.2076(8) 0.3118(8) 0.051(3) Uani 1 1 d . . .
C27 C 0.8523(16) 0.1603(9) 0.2353(9) 0.066(4) Uani 1 1 d . . .
H27A H 0.7880 0.1761 0.1869 0.099 Uiso 1 1 calc R . .
H27B H 0.8475 0.1015 0.2457 0.099 Uiso 1 1 calc R . .
H27C H 0.9285 0.1727 0.2239 0.099 Uiso 1 1 calc R . .
C28 C 0.606(3) 0.359(2) 0.609(2) 0.173(13) Uani 1 1 d . . .
H28A H 0.6702 0.3533 0.5806 0.207 Uiso 1 1 calc R . .
H28B H 0.6110 0.3121 0.6477 0.207 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

































































Ir1 C7 1.994(11) . ?
Ir1 C18 1.996(12) . ?
Ir1 N2 2.014(11) . ?
Ir1 N1 2.049(10) . ?
Ir1 O2 2.140(8) . ?
Ir1 O1 2.158(8) . ?
Br1 C9 1.916(14) . ?
Br2 C20 1.901(16) . ?
O1 C24 1.263(15) . ?
O2 C26 1.298(15) . ?
Cl1 C28 1.78(3) . ?
Cl2 C28 1.66(3) . ?
N1 C1 1.324(17) . ?
N1 C5 1.346(15) . ?
N2 C12 1.342(17) . ?
N2 C16 1.381(16) . ?
C1 C2 1.358(19) . ?
C1 H1 0.9300 . ?
C2 C3 1.40(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.37(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.471(18) . ?
C6 C7 1.395(17) . ?
C6 C11 1.397(17) . ?
C7 C8 1.393(17) . ?
C8 C9 1.361(17) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(19) . ?
C10 C11 1.36(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.38(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.36(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.33(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(19) . ?
C15 H15 0.9300 . ?
C16 C17 1.493(19) . ?
C17 C22 1.365(18) . ?
C17 C18 1.421(18) . ?
C18 C19 1.382(18) . ?
C19 C20 1.415(19) . ?
C19 H19 0.9300 . ?
C20 C21 1.39(2) . ?
C21 C22 1.34(2) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.518(18) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.36(2) . ?
C25 C26 1.38(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.484(19) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 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




















































































































C7 Ir1 C18 90.1(5) . . ?
C7 Ir1 N2 96.7(5) . . ?
C18 Ir1 N2 81.2(5) . . ?
C7 Ir1 N1 80.6(5) . . ?
C18 Ir1 N1 95.6(5) . . ?
N2 Ir1 N1 175.8(4) . . ?
C7 Ir1 O2 90.8(4) . . ?
C18 Ir1 O2 175.4(4) . . ?
N2 Ir1 O2 94.2(4) . . ?
N1 Ir1 O2 89.0(4) . . ?
C7 Ir1 O1 175.1(4) . . ?
C18 Ir1 O1 90.5(4) . . ?
N2 Ir1 O1 88.2(4) . . ?
N1 Ir1 O1 94.5(4) . . ?
O2 Ir1 O1 89.0(3) . . ?
C24 O1 Ir1 123.2(8) . . ?
C26 O2 Ir1 123.7(9) . . ?
C1 N1 C5 120.1(11) . . ?
C1 N1 Ir1 124.2(9) . . ?
C5 N1 Ir1 115.7(9) . . ?
C12 N2 C16 117.1(12) . . ?
C12 N2 Ir1 126.0(9) . . ?
C16 N2 Ir1 116.9(9) . . ?
N1 C1 C2 122.2(14) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C1 C2 C3 119.0(14) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 118.6(14) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 119.4(14) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.6(13) . . ?
N1 C5 C6 113.6(11) . . ?
C4 C5 C6 125.8(12) . . ?
C7 C6 C11 122.2(12) . . ?
C7 C6 C5 115.7(11) . . ?
C11 C6 C5 122.1(12) . . ?
C8 C7 C6 116.6(11) . . ?
C8 C7 Ir1 129.1(9) . . ?
C6 C7 Ir1 114.4(9) . . ?
C9 C8 C7 120.4(12) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 122.9(13) . . ?
C8 C9 Br1 119.9(11) . . ?
C10 C9 Br1 117.2(10) . . ?
C11 C10 C9 118.0(12) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C10 C11 C6 120.0(12) . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
N2 C12 C13 123.5(14) . . ?
N2 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C14 C13 C12 117.7(15) . . ?
C14 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
C15 C14 C13 120.7(14) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 121.0(15) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 N2 120.0(14) . . ?
C15 C16 C17 127.5(13) . . ?
N2 C16 C17 112.4(11) . . ?
C22 C17 C18 120.9(13) . . ?
C22 C17 C16 124.6(12) . . ?
C18 C17 C16 114.5(11) . . ?
C19 C18 C17 117.5(12) . . ?
C19 C18 Ir1 127.7(10) . . ?
C17 C18 Ir1 114.7(9) . . ?
C18 C19 C20 118.5(13) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C21 C20 C19 123.2(15) . . ?
C21 C20 Br2 118.9(11) . . ?
C19 C20 Br2 117.8(12) . . ?
C22 C21 C20 116.1(13) . . ?
C22 C21 H21 121.9 . . ?
C20 C21 H21 121.9 . . ?
C21 C22 C17 123.7(14) . . ?
C21 C22 H22 118.2 . . ?
C17 C22 H22 118.2 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O1 C24 C25 127.9(13) . . ?
O1 C24 C23 113.1(12) . . ?
C25 C24 C23 118.9(13) . . ?
C24 C25 C26 129.7(14) . . ?
C24 C25 H25 115.2 . . ?
C26 C25 H25 115.2 . . ?
O2 C26 C25 126.1(13) . . ?
O2 C26 C27 113.5(12) . . ?
C25 C26 C27 120.4(13) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Cl2 C28 Cl1 111.3(19) . . ?
Cl2 C28 H28A 109.4 . . ?
Cl1 C28 H28A 109.4 . . ?
Cl2 C28 H28B 109.4 . . ?
Cl1 C28 H28B 109.4 . . ?
H28A C28 H28B 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


















































































































C7 Ir1 O1 C24 -85(5) . . . . ?
C18 Ir1 O1 C24 177.9(10) . . . . ?
N2 Ir1 O1 C24 96.7(10) . . . . ?
N1 Ir1 O1 C24 -86.5(10) . . . . ?
O2 Ir1 O1 C24 2.4(9) . . . . ?
C7 Ir1 O2 C26 170.2(10) . . . . ?
C18 Ir1 O2 C26 -88(5) . . . . ?
N2 Ir1 O2 C26 -93.1(10) . . . . ?
N1 Ir1 O2 C26 89.6(10) . . . . ?
O1 Ir1 O2 C26 -5.0(10) . . . . ?
C7 Ir1 N1 C1 179.8(11) . . . . ?
C18 Ir1 N1 C1 90.6(11) . . . . ?
N2 Ir1 N1 C1 130(5) . . . . ?
O2 Ir1 N1 C1 -89.2(10) . . . . ?
O1 Ir1 N1 C1 -0.4(10) . . . . ?
C7 Ir1 N1 C5 0.2(9) . . . . ?
C18 Ir1 N1 C5 -88.9(9) . . . . ?
N2 Ir1 N1 C5 -50(6) . . . . ?
O2 Ir1 N1 C5 91.2(9) . . . . ?
O1 Ir1 N1 C5 -179.9(8) . . . . ?
C7 Ir1 N2 C12 88.1(11) . . . . ?
C18 Ir1 N2 C12 177.1(11) . . . . ?
N1 Ir1 N2 C12 138(5) . . . . ?
O2 Ir1 N2 C12 -3.3(11) . . . . ?
O1 Ir1 N2 C12 -92.1(10) . . . . ?
C7 Ir1 N2 C16 -92.6(9) . . . . ?
C18 Ir1 N2 C16 -3.5(9) . . . . ?
N1 Ir1 N2 C16 -43(6) . . . . ?
O2 Ir1 N2 C16 176.1(8) . . . . ?
O1 Ir1 N2 C16 87.2(9) . . . . ?
C5 N1 C1 C2 0(2) . . . . ?
Ir1 N1 C1 C2 -179.9(11) . . . . ?
N1 C1 C2 C3 3(2) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C1 N1 C5 C4 -2.1(18) . . . . ?
Ir1 N1 C5 C4 177.5(10) . . . . ?
C1 N1 C5 C6 179.8(11) . . . . ?
Ir1 N1 C5 C6 -0.7(13) . . . . ?
C3 C4 C5 N1 2(2) . . . . ?
C3 C4 C5 C6 -179.8(13) . . . . ?
N1 C5 C6 C7 1.0(16) . . . . ?
C4 C5 C6 C7 -177.1(12) . . . . ?
N1 C5 C6 C11 -178.9(12) . . . . ?
C4 C5 C6 C11 3(2) . . . . ?
C11 C6 C7 C8 -0.8(18) . . . . ?
C5 C6 C7 C8 179.3(11) . . . . ?
C11 C6 C7 Ir1 179.1(10) . . . . ?
C5 C6 C7 Ir1 -0.8(14) . . . . ?
C18 Ir1 C7 C8 -84.2(12) . . . . ?
N2 Ir1 C7 C8 -3.0(11) . . . . ?
N1 Ir1 C7 C8 -179.8(12) . . . . ?
O2 Ir1 C7 C8 91.4(11) . . . . ?
O1 Ir1 C7 C8 179(100) . . . . ?
C18 Ir1 C7 C6 95.9(9) . . . . ?
N2 Ir1 C7 C6 177.1(9) . . . . ?
N1 Ir1 C7 C6 0.3(9) . . . . ?
O2 Ir1 C7 C6 -88.5(9) . . . . ?
O1 Ir1 C7 C6 -1(5) . . . . ?
C6 C7 C8 C9 -0.7(18) . . . . ?
Ir1 C7 C8 C9 179.3(10) . . . . ?
C7 C8 C9 C10 2(2) . . . . ?
C7 C8 C9 Br1 -177.8(9) . . . . ?
C8 C9 C10 C11 -2(2) . . . . ?
Br1 C9 C10 C11 178.1(11) . . . . ?
C9 C10 C11 C6 0(2) . . . . ?
C7 C6 C11 C10 1(2) . . . . ?
C5 C6 C11 C10 -179.0(13) . . . . ?
C16 N2 C12 C13 -0.9(19) . . . . ?
Ir1 N2 C12 C13 178.5(11) . . . . ?
N2 C12 C13 C14 0(2) . . . . ?
C12 C13 C14 C15 1(2) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C14 C15 C16 N2 -1(2) . . . . ?
C14 C15 C16 C17 179.3(14) . . . . ?
C12 N2 C16 C15 1.5(18) . . . . ?
Ir1 N2 C16 C15 -177.9(10) . . . . ?
C12 N2 C16 C17 -178.8(11) . . . . ?
Ir1 N2 C16 C17 1.8(13) . . . . ?
C15 C16 C17 C22 1(2) . . . . ?
N2 C16 C17 C22 -178.2(12) . . . . ?
C15 C16 C17 C18 -178.3(13) . . . . ?
N2 C16 C17 C18 2.0(15) . . . . ?
C22 C17 C18 C19 -1.1(18) . . . . ?
C16 C17 C18 C19 178.7(11) . . . . ?
C22 C17 C18 Ir1 175.3(10) . . . . ?
C16 C17 C18 Ir1 -4.9(14) . . . . ?
C7 Ir1 C18 C19 -82.7(12) . . . . ?
N2 Ir1 C18 C19 -179.5(12) . . . . ?
N1 Ir1 C18 C19 -2.1(12) . . . . ?
O2 Ir1 C18 C19 175(5) . . . . ?
O1 Ir1 C18 C19 92.4(11) . . . . ?
C7 Ir1 C18 C17 101.3(10) . . . . ?
N2 Ir1 C18 C17 4.6(9) . . . . ?
N1 Ir1 C18 C17 -178.1(9) . . . . ?
O2 Ir1 C18 C17 0(6) . . . . ?
O1 Ir1 C18 C17 -83.5(9) . . . . ?
C17 C18 C19 C20 -0.8(18) . . . . ?
Ir1 C18 C19 C20 -176.7(10) . . . . ?
C18 C19 C20 C21 3(2) . . . . ?
C18 C19 C20 Br2 -178.7(10) . . . . ?
C19 C20 C21 C22 -3(2) . . . . ?
Br2 C20 C21 C22 178.8(12) . . . . ?
C20 C21 C22 C17 1(2) . . . . ?
C18 C17 C22 C21 1(2) . . . . ?
C16 C17 C22 C21 -178.6(14) . . . . ?
Ir1 O1 C24 C25 2(2) . . . . ?
Ir1 O1 C24 C23 179.9(9) . . . . ?
O1 C24 C25 C26 -7(3) . . . . ?
C23 C24 C25 C26 175.8(15) . . . . ?
Ir1 O2 C26 C25 3(2) . . . . ?
Ir1 O2 C26 C27 -175.7(9) . . . . ?
C24 C25 C26 O2 3(3) . . . . ?
C24 C25 C26 C27 -177.7(15) . . . . ?



_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.996

_refine_diff_density_max         2.943

_refine_diff_density_min         -1.181

_refine_diff_density_rms         0.266

_database_code_depnum_ccdc_archive 'CCDC 981478'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ccc



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C26 H21 Fe N O'

_chemical_formula_weight         419.29



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source










C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Orthorhombic

_symmetry_space_group_name_H-M   Pna2(1)



loop_

_symmetry_equiv_pos_as_xyz




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



_cell_length_a                   30.583(19)

_cell_length_b                   6.321(4)

_cell_length_c                   10.333(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     1997(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    1441

_cell_measurement_theta_min      2.38

_cell_measurement_theta_max      20.01



_exptl_crystal_description       block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.27

_exptl_crystal_size_mid          0.23

_exptl_crystal_size_min          0.19

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.394

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             872

_exptl_absorpt_coefficient_mu    0.772

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.8187

_exptl_absorpt_correction_T_max  0.8672

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            7114

_diffrn_reflns_av_R_equivalents  0.0423

_diffrn_reflns_av_sigmaI/netI    0.0590

_diffrn_reflns_limit_h_min       -26

_diffrn_reflns_limit_h_max       36

_diffrn_reflns_limit_k_min       -6

_diffrn_reflns_limit_k_max       7

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       11

_diffrn_reflns_theta_min         2.38

_diffrn_reflns_theta_max         25.50

_reflns_number_total             3311

_reflns_number_gt                2399

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0323P)²+0.0059P] 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 H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   0.00(3)

_refine_ls_number_reflns         3311

_refine_ls_number_parameters     263

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0643

_refine_ls_R_factor_gt           0.0406

_refine_ls_wR_factor_ref         0.0913

_refine_ls_wR_factor_gt          0.0806

_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_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group


















































C1 C 0.84249(15) 0.0202(6) 1.2377(4) 0.0507(12) Uani 1 1 d . . .
C2 C 0.82617(15) -0.1908(7) 1.2456(4) 0.0570(13) Uani 1 1 d . . .
H2 H 0.8250 -0.2923 1.1740 0.068 Uiso 1 1 calc R . .
C3 C 0.81227(15) -0.2297(8) 1.3733(4) 0.0627(12) Uani 1 1 d . . .
H3 H 0.7996 -0.3620 1.4055 0.075 Uiso 1 1 calc R . .
C4 C 0.81886(15) -0.0453(8) 1.4457(4) 0.0647(13) Uani 1 1 d . . .
H4 H 0.8115 -0.0266 1.5373 0.078 Uiso 1 1 calc R . .
C5 C 0.83719(15) 0.1120(8) 1.3634(4) 0.0576(12) Uani 1 1 d . . .
H5 H 0.8450 0.2567 1.3884 0.069 Uiso 1 1 calc R . .
C6 C 0.74540(19) 0.1733(14) 1.1573(6) 0.0936(19) Uani 1 1 d . . .
H6 H 0.7580 0.2413 1.0807 0.112 Uiso 1 1 calc R . .
C7 C 0.7388(2) 0.2675(9) 1.2768(10) 0.104(2) Uani 1 1 d . . .
H7 H 0.7460 0.4137 1.2999 0.125 Uiso 1 1 calc R . .
C8 C 0.7195(2) 0.1230(16) 1.3546(6) 0.108(2) Uani 1 1 d . . .
H8 H 0.7108 0.1453 1.4447 0.129 Uiso 1 1 calc R . .
C9 C 0.71422(16) -0.0616(10) 1.2842(12) 0.0942(17) Uani 1 1 d . . .
H9 H 0.7011 -0.1930 1.3164 0.113 Uiso 1 1 calc R . .
C10 C 0.7297(2) -0.0299(12) 1.1639(7) 0.0918(19) Uani 1 1 d . . .
H10 H 0.7297 -0.1334 1.0932 0.110 Uiso 1 1 calc R . .
C11 C 0.85917(13) 0.1225(6) 1.1219(4) 0.0459(10) Uani 1 1 d . . .
C12 C 0.87432(13) 0.3339(6) 1.1253(4) 0.0560(11) Uani 1 1 d . . .
H12 H 0.8731 0.4095 1.2024 0.067 Uiso 1 1 calc R . .
C13 C 0.89034(15) 0.4261(6) 1.0189(4) 0.0563(11) Uani 1 1 d . . .
H13 H 0.9000 0.5655 1.0218 0.068 Uiso 1 1 calc R . .
C14 C 0.89244(13) 0.3107(6) 0.9020(4) 0.0448(10) Uani 1 1 d . . .
C15 C 0.90997(11) 0.3907(5) 0.7865(5) 0.0480(9) Uani 1 1 d . . .
H15 H 0.9198 0.5298 0.7841 0.058 Uiso 1 1 calc R . .
C16 C 0.91290(12) 0.2685(6) 0.6772(4) 0.0445(10) Uani 1 1 d . . .
C17 C 0.89704(14) 0.0604(6) 0.6823(4) 0.0494(11) Uani 1 1 d . . .
H17 H 0.8992 -0.0243 0.6090 0.059 Uiso 1 1 calc R . .
C18 C 0.87872(11) -0.0207(5) 0.7905(6) 0.0480(8) Uani 1 1 d . . .
H18 H 0.8675 -0.1574 0.7893 0.058 Uiso 1 1 calc R . .
C19 C 0.87652(12) 0.1000(6) 0.9051(4) 0.0420(9) Uani 1 1 d . . .
C20 C 0.93222(14) 0.3525(6) 0.5566(4) 0.0487(10) Uani 1 1 d . . .
C21 C 0.91646(16) 0.5355(7) 0.5007(5) 0.0640(13) Uani 1 1 d . . .
H21 H 0.8933 0.6059 0.5402 0.077 Uiso 1 1 calc R . .
C22 C 0.93380(19) 0.6172(9) 0.3887(5) 0.0834(15) Uani 1 1 d . . .
H22 H 0.9225 0.7412 0.3535 0.100 Uiso 1 1 calc R . .
C23 C 0.9680(2) 0.5143(9) 0.3289(5) 0.0916(19) Uani 1 1 d . . .
H23 H 0.9800 0.5690 0.2532 0.110 Uiso 1 1 calc R . .
C24 C 0.98464(17) 0.3291(9) 0.3818(5) 0.0823(15) Uani 1 1 d . . .
H24 H 1.0073 0.2576 0.3408 0.099 Uiso 1 1 calc R . .
C25 C 0.96724(16) 0.2517(8) 0.4957(5) 0.0660(12) Uani 1 1 d . . .
C26 C 1.0207(2) -0.0242(9) 0.5124(8) 0.116(3) Uani 1 1 d . . .
H26A H 1.0164 -0.0666 0.4241 0.175 Uiso 1 1 calc R . .
H26B H 1.0266 -0.1466 0.5645 0.175 Uiso 1 1 calc R . .
H26C H 1.0450 0.0718 0.5174 0.175 Uiso 1 1 calc R . .
Fe1 Fe 0.778501(16) 0.01578(8) 1.29345(10) 0.04957(17) Uani 1 1 d . . .
N1 N 0.86000(11) 0.0096(5) 1.0149(3) 0.0481(8) Uani 1 1 d . . .
O1 O 0.98248(13) 0.0774(7) 0.5585(4) 0.0867(12) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag






























































C1 C2 1.427(5) . ?
C1 C5 1.431(6) . ?
C1 C11 1.453(6) . ?
C1 Fe1 2.040(5) . ?
C2 C3 1.408(6) . ?
C2 Fe1 2.018(5) . ?
C2 H2 0.9800 . ?
C3 C4 1.400(6) . ?
C3 Fe1 2.039(5) . ?
C3 H3 0.9800 . ?
C4 C5 1.424(6) . ?
C4 Fe1 2.037(4) . ?
C4 H4 0.9800 . ?
C5 Fe1 2.028(5) . ?
C5 H5 0.9800 . ?
C6 C10 1.373(7) . ?
C6 C7 1.385(8) . ?
C6 Fe1 1.999(5) . ?
C6 H6 0.9800 . ?
C7 C8 1.352(8) . ?
C7 Fe1 2.008(5) . ?
C7 H7 0.9800 . ?
C8 C9 1.385(10) . ?
C8 Fe1 2.027(6) . ?
C8 H8 0.9800 . ?
C9 C10 1.346(11) . ?
C9 Fe1 2.028(5) . ?
C9 H9 0.9800 . ?
C10 Fe1 2.026(5) . ?
C10 H10 0.9800 . ?
C11 N1 1.316(5) . ?
C11 C12 1.415(5) . ?
C12 C13 1.338(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.413(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.402(6) . ?
C14 C19 1.419(5) . ?
C15 C16 1.372(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(5) . ?
C16 C20 1.478(5) . ?
C17 C18 1.352(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.411(6) . ?
C18 H18 0.9300 . ?
C19 N1 1.367(5) . ?
C20 C21 1.380(6) . ?
C20 C25 1.396(6) . ?
C21 C22 1.374(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.379(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.388(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.381(6) . ?
C24 H24 0.9300 . ?
C25 O1 1.361(6) . ?
C26 O1 1.416(5) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?



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 C1 C5 106.7(4) . . ?
C2 C1 C11 125.9(4) . . ?
C5 C1 C11 127.4(4) . . ?
C2 C1 Fe1 68.6(3) . . ?
C5 C1 Fe1 68.9(3) . . ?
C11 C1 Fe1 125.1(3) . . ?
C3 C2 C1 108.8(4) . . ?
C3 C2 Fe1 70.5(3) . . ?
C1 C2 Fe1 70.2(2) . . ?
C3 C2 H2 125.6 . . ?
C1 C2 H2 125.6 . . ?
Fe1 C2 H2 125.6 . . ?
C4 C3 C2 108.2(4) . . ?
C4 C3 Fe1 69.8(3) . . ?
C2 C3 Fe1 68.9(3) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
Fe1 C3 H3 125.9 . . ?
C3 C4 C5 108.6(4) . . ?
C3 C4 Fe1 70.0(3) . . ?
C5 C4 Fe1 69.2(3) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Fe1 C4 H4 125.7 . . ?
C4 C5 C1 107.7(4) . . ?
C4 C5 Fe1 69.8(3) . . ?
C1 C5 Fe1 69.9(3) . . ?
C4 C5 H5 126.2 . . ?
C1 C5 H5 126.2 . . ?
Fe1 C5 H5 126.2 . . ?
C10 C6 C7 107.9(6) . . ?
C10 C6 Fe1 71.1(3) . . ?
C7 C6 Fe1 70.2(3) . . ?
C10 C6 H6 126.0 . . ?
C7 C6 H6 126.0 . . ?
Fe1 C6 H6 126.0 . . ?
C8 C7 C6 107.6(6) . . ?
C8 C7 Fe1 71.2(3) . . ?
C6 C7 Fe1 69.4(3) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
Fe1 C7 H7 126.2 . . ?
C7 C8 C9 108.0(7) . . ?
C7 C8 Fe1 69.7(3) . . ?
C9 C8 Fe1 70.1(3) . . ?
C7 C8 H8 126.0 . . ?
C9 C8 H8 126.0 . . ?
Fe1 C8 H8 126.0 . . ?
C10 C9 C8 108.5(7) . . ?
C10 C9 Fe1 70.5(4) . . ?
C8 C9 Fe1 70.0(3) . . ?
C10 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
Fe1 C9 H9 125.7 . . ?
C9 C10 C6 107.9(6) . . ?
C9 C10 Fe1 70.7(3) . . ?
C6 C10 Fe1 69.0(3) . . ?
C9 C10 H10 126.0 . . ?
C6 C10 H10 126.0 . . ?
Fe1 C10 H10 126.0 . . ?
N1 C11 C12 121.8(4) . . ?
N1 C11 C1 117.2(4) . . ?
C12 C11 C1 121.0(4) . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 124.0(4) . . ?
C15 C14 C19 119.3(3) . . ?
C13 C14 C19 116.7(4) . . ?
C16 C15 C14 121.5(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 118.3(4) . . ?
C15 C16 C20 121.2(4) . . ?
C17 C16 C20 120.5(4) . . ?
C18 C17 C16 122.0(4) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C17 C18 C19 120.6(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
N1 C19 C18 119.2(4) . . ?
N1 C19 C14 122.6(3) . . ?
C18 C19 C14 118.2(4) . . ?
C21 C20 C25 117.5(4) . . ?
C21 C20 C16 121.0(4) . . ?
C25 C20 C16 121.5(4) . . ?
C22 C21 C20 122.2(5) . . ?
C22 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C21 C22 C23 119.5(5) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C24 120.0(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.6(5) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
O1 C25 C24 124.2(5) . . ?
O1 C25 C20 114.7(4) . . ?
C24 C25 C20 121.2(5) . . ?
O1 C26 H26A 109.5 . . ?
O1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C6 Fe1 C7 40.4(2) . . ?
C6 Fe1 C2 121.0(3) . . ?
C7 Fe1 C2 158.1(3) . . ?
C6 Fe1 C10 39.9(2) . . ?
C7 Fe1 C10 67.1(3) . . ?
C2 Fe1 C10 106.1(2) . . ?
C6 Fe1 C9 66.2(3) . . ?
C7 Fe1 C9 66.5(2) . . ?
C2 Fe1 C9 122.2(2) . . ?
C10 Fe1 C9 38.8(3) . . ?
C6 Fe1 C8 66.5(3) . . ?
C7 Fe1 C8 39.1(2) . . ?
C2 Fe1 C8 159.2(3) . . ?
C10 Fe1 C8 66.3(3) . . ?
C9 Fe1 C8 39.9(3) . . ?
C6 Fe1 C5 123.3(3) . . ?
C7 Fe1 C5 109.1(2) . . ?
C2 Fe1 C5 69.02(19) . . ?
C10 Fe1 C5 158.5(3) . . ?
C9 Fe1 C5 161.3(4) . . ?
C8 Fe1 C5 125.2(3) . . ?
C6 Fe1 C4 160.9(3) . . ?
C7 Fe1 C4 125.6(3) . . ?
C2 Fe1 C4 68.22(18) . . ?
C10 Fe1 C4 158.4(3) . . ?
C9 Fe1 C4 125.3(3) . . ?
C8 Fe1 C4 111.2(2) . . ?
C5 Fe1 C4 41.01(18) . . ?
C6 Fe1 C3 157.0(3) . . ?
C7 Fe1 C3 160.7(3) . . ?
C2 Fe1 C3 40.62(16) . . ?
C10 Fe1 C3 122.2(3) . . ?
C9 Fe1 C3 109.0(2) . . ?
C8 Fe1 C3 125.4(3) . . ?
C5 Fe1 C3 68.6(2) . . ?
C4 Fe1 C3 40.17(18) . . ?
C6 Fe1 C1 106.3(2) . . ?
C7 Fe1 C1 123.0(3) . . ?
C2 Fe1 C1 41.15(15) . . ?
C10 Fe1 C1 121.5(2) . . ?
C9 Fe1 C1 156.9(3) . . ?
C8 Fe1 C1 159.5(3) . . ?
C5 Fe1 C1 41.19(16) . . ?
C4 Fe1 C1 68.87(19) . . ?
C3 Fe1 C1 68.83(17) . . ?
C11 N1 C19 118.5(3) . . ?
C25 O1 C26 119.3(4) . . ?



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
























































































































































































































































C5 C1 C2 C3 -1.5(5) . . . . ?
C11 C1 C2 C3 -178.8(4) . . . . ?
Fe1 C1 C2 C3 -60.1(3) . . . . ?
C5 C1 C2 Fe1 58.6(3) . . . . ?
C11 C1 C2 Fe1 -118.6(4) . . . . ?
C1 C2 C3 C4 1.0(5) . . . . ?
Fe1 C2 C3 C4 -59.0(3) . . . . ?
C1 C2 C3 Fe1 60.0(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
Fe1 C3 C4 C5 -58.5(3) . . . . ?
C2 C3 C4 Fe1 58.4(3) . . . . ?
C3 C4 C5 C1 -0.8(5) . . . . ?
Fe1 C4 C5 C1 -59.9(3) . . . . ?
C3 C4 C5 Fe1 59.0(3) . . . . ?
C2 C1 C5 C4 1.4(5) . . . . ?
C11 C1 C5 C4 178.6(4) . . . . ?
Fe1 C1 C5 C4 59.8(3) . . . . ?
C2 C1 C5 Fe1 -58.4(3) . . . . ?
C11 C1 C5 Fe1 118.8(5) . . . . ?
C10 C6 C7 C8 0.2(7) . . . . ?
Fe1 C6 C7 C8 -61.3(4) . . . . ?
C10 C6 C7 Fe1 61.4(4) . . . . ?
C6 C7 C8 C9 0.3(7) . . . . ?
Fe1 C7 C8 C9 -59.9(4) . . . . ?
C6 C7 C8 Fe1 60.1(4) . . . . ?
C7 C8 C9 C10 -0.6(7) . . . . ?
Fe1 C8 C9 C10 -60.2(4) . . . . ?
C7 C8 C9 Fe1 59.6(5) . . . . ?
C8 C9 C10 C6 0.7(7) . . . . ?
Fe1 C9 C10 C6 -59.2(4) . . . . ?
C8 C9 C10 Fe1 59.9(4) . . . . ?
C7 C6 C10 C9 -0.6(7) . . . . ?
Fe1 C6 C10 C9 60.3(4) . . . . ?
C7 C6 C10 Fe1 -60.8(4) . . . . ?
C2 C1 C11 N1 -1.2(6) . . . . ?
C5 C1 C11 N1 -177.9(4) . . . . ?
Fe1 C1 C11 N1 -88.8(4) . . . . ?
C2 C1 C11 C12 179.6(4) . . . . ?
C5 C1 C11 C12 2.8(7) . . . . ?
Fe1 C1 C11 C12 92.0(5) . . . . ?
N1 C11 C12 C13 -0.3(6) . . . . ?
C1 C11 C12 C13 178.8(4) . . . . ?
C11 C12 C13 C14 -0.5(6) . . . . ?
C12 C13 C14 C15 -177.8(4) . . . . ?
C12 C13 C14 C19 0.7(6) . . . . ?
C13 C14 C15 C16 177.2(4) . . . . ?
C19 C14 C15 C16 -1.3(6) . . . . ?
C14 C15 C16 C17 1.2(6) . . . . ?
C14 C15 C16 C20 -178.8(3) . . . . ?
C15 C16 C17 C18 0.8(6) . . . . ?
C20 C16 C17 C18 -179.2(4) . . . . ?
C16 C17 C18 C19 -2.6(6) . . . . ?
C17 C18 C19 N1 -176.4(3) . . . . ?
C17 C18 C19 C14 2.5(6) . . . . ?
C15 C14 C19 N1 178.3(3) . . . . ?
C13 C14 C19 N1 -0.3(6) . . . . ?
C15 C14 C19 C18 -0.5(5) . . . . ?
C13 C14 C19 C18 -179.1(4) . . . . ?
C15 C16 C20 C21 -55.3(6) . . . . ?
C17 C16 C20 C21 124.6(4) . . . . ?
C15 C16 C20 C25 124.0(4) . . . . ?
C17 C16 C20 C25 -56.0(6) . . . . ?
C25 C20 C21 C22 0.6(7) . . . . ?
C16 C20 C21 C22 180.0(4) . . . . ?
C20 C21 C22 C23 0.2(8) . . . . ?
C21 C22 C23 C24 0.2(8) . . . . ?
C22 C23 C24 C25 -1.3(8) . . . . ?
C23 C24 C25 O1 -176.8(5) . . . . ?
C23 C24 C25 C20 2.2(7) . . . . ?
C21 C20 C25 O1 177.3(4) . . . . ?
C16 C20 C25 O1 -2.1(6) . . . . ?
C21 C20 C25 C24 -1.8(6) . . . . ?
C16 C20 C25 C24 178.9(4) . . . . ?
C10 C6 Fe1 C7 -118.0(6) . . . . ?
C10 C6 Fe1 C2 77.6(4) . . . . ?
C7 C6 Fe1 C2 -164.4(4) . . . . ?
C7 C6 Fe1 C10 118.0(6) . . . . ?
C10 C6 Fe1 C9 -36.8(4) . . . . ?
C7 C6 Fe1 C9 81.2(5) . . . . ?
C10 C6 Fe1 C8 -80.6(4) . . . . ?
C7 C6 Fe1 C8 37.4(4) . . . . ?
C10 C6 Fe1 C5 161.6(4) . . . . ?
C7 C6 Fe1 C5 -80.4(4) . . . . ?
C10 C6 Fe1 C4 -167.8(6) . . . . ?
C7 C6 Fe1 C4 -49.9(8) . . . . ?
C10 C6 Fe1 C3 45.9(7) . . . . ?
C7 C6 Fe1 C3 163.8(5) . . . . ?
C10 C6 Fe1 C1 119.9(4) . . . . ?
C7 C6 Fe1 C1 -122.1(4) . . . . ?
C8 C7 Fe1 C6 118.0(6) . . . . ?
C8 C7 Fe1 C2 156.1(6) . . . . ?
C6 C7 Fe1 C2 38.1(8) . . . . ?
C8 C7 Fe1 C10 80.1(5) . . . . ?
C6 C7 Fe1 C10 -37.9(4) . . . . ?
C8 C7 Fe1 C9 37.8(5) . . . . ?
C6 C7 Fe1 C9 -80.3(5) . . . . ?
C6 C7 Fe1 C8 -118.0(6) . . . . ?
C8 C7 Fe1 C5 -122.7(5) . . . . ?
C6 C7 Fe1 C5 119.3(4) . . . . ?
C8 C7 Fe1 C4 -79.9(5) . . . . ?
C6 C7 Fe1 C4 162.1(4) . . . . ?
C8 C7 Fe1 C3 -42.8(9) . . . . ?
C6 C7 Fe1 C3 -160.8(6) . . . . ?
C8 C7 Fe1 C1 -166.2(4) . . . . ?
C6 C7 Fe1 C1 75.7(5) . . . . ?
C3 C2 Fe1 C6 -161.6(4) . . . . ?
C1 C2 Fe1 C6 79.0(4) . . . . ?
C3 C2 Fe1 C7 170.5(6) . . . . ?
C1 C2 Fe1 C7 51.1(7) . . . . ?
C3 C2 Fe1 C10 -120.9(3) . . . . ?
C1 C2 Fe1 C10 119.7(3) . . . . ?
C3 C2 Fe1 C9 -81.9(4) . . . . ?
C1 C2 Fe1 C9 158.7(4) . . . . ?
C3 C2 Fe1 C8 -55.5(7) . . . . ?
C1 C2 Fe1 C8 -175.0(6) . . . . ?
C3 C2 Fe1 C5 81.2(3) . . . . ?
C1 C2 Fe1 C5 -38.2(2) . . . . ?
C3 C2 Fe1 C4 37.1(3) . . . . ?
C1 C2 Fe1 C4 -82.4(3) . . . . ?
C1 C2 Fe1 C3 -119.4(4) . . . . ?
C3 C2 Fe1 C1 119.4(4) . . . . ?
C9 C10 Fe1 C6 -118.9(6) . . . . ?
C9 C10 Fe1 C7 -80.5(4) . . . . ?
C6 C10 Fe1 C7 38.5(4) . . . . ?
C9 C10 Fe1 C2 121.7(4) . . . . ?
C6 C10 Fe1 C2 -119.4(4) . . . . ?
C6 C10 Fe1 C9 118.9(6) . . . . ?
C9 C10 Fe1 C8 -37.7(4) . . . . ?
C6 C10 Fe1 C8 81.2(4) . . . . ?
C9 C10 Fe1 C5 -164.7(5) . . . . ?
C6 C10 Fe1 C5 -45.8(8) . . . . ?
C9 C10 Fe1 C4 50.3(8) . . . . ?
C6 C10 Fe1 C4 169.2(5) . . . . ?
C9 C10 Fe1 C3 80.4(5) . . . . ?
C6 C10 Fe1 C3 -160.7(4) . . . . ?
C9 C10 Fe1 C1 163.8(4) . . . . ?
C6 C10 Fe1 C1 -77.3(4) . . . . ?
C10 C9 Fe1 C6 37.8(4) . . . . ?
C8 C9 Fe1 C6 -81.4(5) . . . . ?
C10 C9 Fe1 C7 82.2(5) . . . . ?
C8 C9 Fe1 C7 -37.0(4) . . . . ?
C10 C9 Fe1 C2 -75.0(5) . . . . ?
C8 C9 Fe1 C2 165.8(4) . . . . ?
C8 C9 Fe1 C10 -119.2(7) . . . . ?
C10 C9 Fe1 C8 119.2(7) . . . . ?
C10 C9 Fe1 C5 162.5(7) . . . . ?
C8 C9 Fe1 C5 43.3(10) . . . . ?
C10 C9 Fe1 C4 -159.7(4) . . . . ?
C8 C9 Fe1 C4 81.1(5) . . . . ?
C10 C9 Fe1 C3 -118.0(4) . . . . ?
C8 C9 Fe1 C3 122.8(5) . . . . ?
C10 C9 Fe1 C1 -37.4(8) . . . . ?
C8 C9 Fe1 C1 -156.6(5) . . . . ?
C7 C8 Fe1 C6 -38.6(4) . . . . ?
C9 C8 Fe1 C6 80.3(5) . . . . ?
C9 C8 Fe1 C7 119.0(7) . . . . ?
C7 C8 Fe1 C2 -154.8(7) . . . . ?
C9 C8 Fe1 C2 -35.8(9) . . . . ?
C7 C8 Fe1 C10 -82.3(5) . . . . ?
C9 C8 Fe1 C10 36.7(5) . . . . ?
C7 C8 Fe1 C9 -119.0(7) . . . . ?
C7 C8 Fe1 C5 76.7(5) . . . . ?
C9 C8 Fe1 C5 -164.4(5) . . . . ?
C7 C8 Fe1 C4 120.9(5) . . . . ?
C9 C8 Fe1 C4 -120.2(5) . . . . ?
C7 C8 Fe1 C3 164.0(4) . . . . ?
C9 C8 Fe1 C3 -77.0(6) . . . . ?
C7 C8 Fe1 C1 34.7(9) . . . . ?
C9 C8 Fe1 C1 153.7(7) . . . . ?
C4 C5 Fe1 C6 165.4(3) . . . . ?
C1 C5 Fe1 C6 -76.0(4) . . . . ?
C4 C5 Fe1 C7 122.7(4) . . . . ?
C1 C5 Fe1 C7 -118.6(4) . . . . ?
C4 C5 Fe1 C2 -80.5(3) . . . . ?
C1 C5 Fe1 C2 38.1(2) . . . . ?
C4 C5 Fe1 C10 -161.3(6) . . . . ?
C1 C5 Fe1 C10 -42.6(7) . . . . ?
C4 C5 Fe1 C9 49.6(9) . . . . ?
C1 C5 Fe1 C9 168.3(7) . . . . ?
C4 C5 Fe1 C8 82.2(4) . . . . ?
C1 C5 Fe1 C8 -159.1(4) . . . . ?
C1 C5 Fe1 C4 118.7(4) . . . . ?
C4 C5 Fe1 C3 -36.8(3) . . . . ?
C1 C5 Fe1 C3 81.8(3) . . . . ?
C4 C5 Fe1 C1 -118.7(4) . . . . ?
C3 C4 Fe1 C6 -160.4(6) . . . . ?
C5 C4 Fe1 C6 -40.3(8) . . . . ?
C3 C4 Fe1 C7 162.0(4) . . . . ?
C5 C4 Fe1 C7 -77.9(4) . . . . ?
C3 C4 Fe1 C2 -37.5(3) . . . . ?
C5 C4 Fe1 C2 82.6(3) . . . . ?
C3 C4 Fe1 C10 41.2(7) . . . . ?
C5 C4 Fe1 C10 161.3(6) . . . . ?
C3 C4 Fe1 C9 77.4(4) . . . . ?
C5 C4 Fe1 C9 -162.5(4) . . . . ?
C3 C4 Fe1 C8 120.2(4) . . . . ?
C5 C4 Fe1 C8 -119.7(4) . . . . ?
C3 C4 Fe1 C5 -120.1(4) . . . . ?
C5 C4 Fe1 C3 120.1(4) . . . . ?
C3 C4 Fe1 C1 -81.8(3) . . . . ?
C5 C4 Fe1 C1 38.3(3) . . . . ?
C4 C3 Fe1 C6 163.7(5) . . . . ?
C2 C3 Fe1 C6 43.8(7) . . . . ?
C4 C3 Fe1 C7 -49.5(8) . . . . ?
C2 C3 Fe1 C7 -169.3(6) . . . . ?
C4 C3 Fe1 C2 119.8(4) . . . . ?
C4 C3 Fe1 C10 -163.4(3) . . . . ?
C2 C3 Fe1 C10 76.8(4) . . . . ?
C4 C3 Fe1 C9 -122.6(4) . . . . ?
C2 C3 Fe1 C9 117.6(4) . . . . ?
C4 C3 Fe1 C8 -81.2(4) . . . . ?
C2 C3 Fe1 C8 159.0(4) . . . . ?
C4 C3 Fe1 C5 37.6(3) . . . . ?
C2 C3 Fe1 C5 -82.3(3) . . . . ?
C2 C3 Fe1 C4 -119.8(4) . . . . ?
C4 C3 Fe1 C1 81.9(3) . . . . ?
C2 C3 Fe1 C1 -37.9(3) . . . . ?
C2 C1 Fe1 C6 -118.8(4) . . . . ?
C5 C1 Fe1 C6 122.4(4) . . . . ?
C11 C1 Fe1 C6 0.8(5) . . . . ?
C2 C1 Fe1 C7 -159.7(4) . . . . ?
C5 C1 Fe1 C7 81.5(4) . . . . ?
C11 C1 Fe1 C7 -40.1(5) . . . . ?
C5 C1 Fe1 C2 -118.8(3) . . . . ?
C11 C1 Fe1 C2 119.6(5) . . . . ?
C2 C1 Fe1 C10 -78.2(4) . . . . ?
C5 C1 Fe1 C10 163.1(3) . . . . ?
C11 C1 Fe1 C10 41.4(5) . . . . ?
C2 C1 Fe1 C9 -51.7(7) . . . . ?
C5 C1 Fe1 C9 -170.4(7) . . . . ?
C11 C1 Fe1 C9 67.9(7) . . . . ?
C2 C1 Fe1 C8 174.9(6) . . . . ?
C5 C1 Fe1 C8 56.1(7) . . . . ?
C11 C1 Fe1 C8 -65.5(8) . . . . ?
C2 C1 Fe1 C5 118.8(3) . . . . ?
C11 C1 Fe1 C5 -121.6(5) . . . . ?
C2 C1 Fe1 C4 80.7(3) . . . . ?
C5 C1 Fe1 C4 -38.1(3) . . . . ?
C11 C1 Fe1 C4 -159.7(4) . . . . ?
C2 C1 Fe1 C3 37.4(2) . . . . ?
C5 C1 Fe1 C3 -81.3(3) . . . . ?
C11 C1 Fe1 C3 157.0(4) . . . . ?
C12 C11 N1 C19 0.8(6) . . . . ?
C1 C11 N1 C19 -178.4(4) . . . . ?
C18 C19 N1 C11 178.3(3) . . . . ?
C14 C19 N1 C11 -0.5(5) . . . . ?
C24 C25 O1 C26 5.4(7) . . . . ?
C20 C25 O1 C26 -173.6(4) . . . . ?



_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.185

_refine_diff_density_min         -0.302

_refine_diff_density_rms         0.042

_database_code_depnum_ccdc_archive 'CCDC 992168'
