# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_rda004
_database_code_depnum_ccdc_archive 'CCDC 1518956'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2012-05-12T21:35:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C31 H33 B F4 N4 O2'
_chemical_formula_moiety         'C31 H33 N4 O2, B F4'
_chemical_formula_weight         580.42

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-p 2ybc'
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                   13.1990(6)
_cell_length_b                   12.1266(4)
_cell_length_c                   18.1368(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.542(4)
_cell_angle_gamma                90
_cell_volume                     2752.27(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2762
_cell_measurement_theta_min      3.6569
_cell_measurement_theta_max      30.7093

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
      CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.9293
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      0.0200093
_diffrn_orient_matrix_ub_12      -0.0471753
_diffrn_orient_matrix_ub_13      -0.0138887
_diffrn_orient_matrix_ub_21      0.00471
_diffrn_orient_matrix_ub_22      0.0310872
_diffrn_orient_matrix_ub_23      -0.0318801
_diffrn_orient_matrix_ub_31      0.052827
_diffrn_orient_matrix_ub_32      0.0151102
_diffrn_orient_matrix_ub_33      0.0222093
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_number            13629
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.66
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_reflns_number_total             6534
_reflns_number_gt                3814
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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)+(0.0368P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6534
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1324
_refine_ls_wR_factor_gt          0.1104
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.066

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.77741(19) 0.59593(18) 0.18942(13) 0.0160(5) Uani 1 1 d . . .
H1 H 0.84 0.58 0.1763 0.019 Uiso 1 1 calc R . .
N2 N 0.77763(15) 0.66369(15) 0.24630(10) 0.0148(4) Uani 1 1 d . . .
C3 C 0.67280(18) 0.65272(19) 0.26051(13) 0.0174(5) Uani 1 1 d . . .
H3A H 0.6444 0.7255 0.269 0.021 Uiso 1 1 calc R . .
H3B H 0.6786 0.6047 0.3058 0.021 Uiso 1 1 calc R . .
C4 C 0.60276(18) 0.5995(2) 0.18426(13) 0.0192(5) Uani 1 1 d . . .
H4A H 0.5562 0.5413 0.1942 0.023 Uiso 1 1 calc R . .
H4B H 0.558 0.6552 0.1486 0.023 Uiso 1 1 calc R . .
N5 N 0.68478(15) 0.55230(15) 0.15249(10) 0.0154(4) Uani 1 1 d . . .
C21 C 0.87670(17) 0.68983(19) 0.30531(12) 0.0146(5) Uani 1 1 d . . .
C22 C 0.94354(18) 0.60376(18) 0.33982(12) 0.0146(5) Uani 1 1 d . . .
N221 N 0.90337(15) 0.49318(15) 0.32486(10) 0.0154(4) Uani 1 1 d . . .
C122 C 0.87248(19) 0.45069(19) 0.39100(13) 0.0186(5) Uani 1 1 d . . .
H22A H 0.8234 0.5032 0.4042 0.022 Uiso 1 1 calc R . .
H22B H 0.9367 0.4418 0.4372 0.022 Uiso 1 1 calc R . .
C223 C 0.8178(2) 0.34063(19) 0.36813(14) 0.0217(6) Uani 1 1 d . . .
H22C H 0.7973 0.3106 0.4121 0.026 Uiso 1 1 calc R . .
H22D H 0.7518 0.351 0.3236 0.026 Uiso 1 1 calc R . .
O224 O 0.88599(13) 0.26398(13) 0.34726(10) 0.0246(4) Uani 1 1 d . . .
C225 C 0.9173(2) 0.30609(19) 0.28423(14) 0.0234(6) Uani 1 1 d . . .
H22E H 0.8531 0.316 0.2382 0.028 Uiso 1 1 calc R . .
H22F H 0.9647 0.2522 0.2706 0.028 Uiso 1 1 calc R . .
C226 C 0.97509(19) 0.41546(18) 0.30501(14) 0.0196(5) Uani 1 1 d . . .
H22G H 1.041 0.4059 0.3498 0.024 Uiso 1 1 calc R . .
H22H H 0.9953 0.4436 0.2604 0.024 Uiso 1 1 calc R . .
C23 C 1.04684(18) 0.62880(19) 0.39283(13) 0.0170(5) Uani 1 1 d . . .
H23 H 1.0954 0.5708 0.415 0.02 Uiso 1 1 calc R . .
C24 C 1.07586(19) 0.7354(2) 0.41160(13) 0.0192(5) Uani 1 1 d . . .
H24 H 1.1455 0.7507 0.4458 0.023 Uiso 1 1 calc R . .
C24A C 1.00523(18) 0.82396(19) 0.38161(13) 0.0161(5) Uani 1 1 d . . .
C25 C 1.03157(19) 0.93447(19) 0.40546(13) 0.0206(6) Uani 1 1 d . . .
H25 H 1.0989 0.9506 0.4427 0.025 Uiso 1 1 calc R . .
C26 C 0.96094(19) 1.0184(2) 0.37532(14) 0.0217(6) Uani 1 1 d . . .
H26 H 0.9794 1.0918 0.3927 0.026 Uiso 1 1 calc R . .
C27 C 0.86109(19) 0.9972(2) 0.31882(14) 0.0209(6) Uani 1 1 d . . .
H27 H 0.8134 1.0563 0.298 0.025 Uiso 1 1 calc R . .
C28 C 0.83275(18) 0.89095(18) 0.29386(13) 0.0157(5) Uani 1 1 d . . .
H28 H 0.7658 0.8772 0.2554 0.019 Uiso 1 1 calc R . .
C28A C 0.90329(18) 0.80170(19) 0.32539(13) 0.0156(5) Uani 1 1 d . . .
C51 C 0.66672(18) 0.49003(19) 0.08178(13) 0.0165(5) Uani 1 1 d . . .
C52 C 0.68890(18) 0.53761(19) 0.01890(13) 0.0179(5) Uani 1 1 d . . .
N521 N 0.73084(15) 0.64660(15) 0.02492(11) 0.0169(4) Uani 1 1 d . . .
C522 C 0.65479(19) 0.73758(19) 0.02022(15) 0.0233(6) Uani 1 1 d . . .
H52A H 0.6111 0.7215 0.0543 0.028 Uiso 1 1 calc R . .
H52B H 0.6062 0.7447 -0.0338 0.028 Uiso 1 1 calc R . .
C523 C 0.7155(2) 0.8442(2) 0.04537(16) 0.0296(7) Uani 1 1 d . . .
H52C H 0.664 0.9055 0.0397 0.035 Uiso 1 1 calc R . .
H52D H 0.7586 0.8389 0.101 0.035 Uiso 1 1 calc R . .
O524 O 0.78453(14) 0.86825(13) 0.00051(10) 0.0274(4) Uani 1 1 d . . .
C525 C 0.85421(19) 0.7784(2) 0.00256(14) 0.0210(6) Uani 1 1 d . . .
H52E H 0.9017 0.7676 0.0566 0.025 Uiso 1 1 calc R . .
H52F H 0.8996 0.7961 -0.03 0.025 Uiso 1 1 calc R . .
C526 C 0.79419(19) 0.67328(19) -0.02620(13) 0.0193(5) Uani 1 1 d . . .
H52G H 0.7466 0.6828 -0.0804 0.023 Uiso 1 1 calc R . .
H52H H 0.8449 0.6128 -0.0252 0.023 Uiso 1 1 calc R . .
C53 C 0.67679(18) 0.4717(2) -0.04745(13) 0.0196(5) Uani 1 1 d . . .
H53 H 0.6868 0.5039 -0.0924 0.023 Uiso 1 1 calc R . .
C54 C 0.65095(18) 0.3626(2) -0.04849(13) 0.0188(5) Uani 1 1 d . . .
H54 H 0.6446 0.3202 -0.0938 0.023 Uiso 1 1 calc R . .
C54A C 0.63338(18) 0.31137(19) 0.01642(13) 0.0172(5) Uani 1 1 d . . .
C55 C 0.61362(18) 0.1958(2) 0.01779(14) 0.0212(6) Uani 1 1 d . . .
H55 H 0.6104 0.1515 -0.0261 0.025 Uiso 1 1 calc R . .
C56 C 0.59941(19) 0.1487(2) 0.08210(15) 0.0251(6) Uani 1 1 d . . .
H56 H 0.5872 0.0716 0.0829 0.03 Uiso 1 1 calc R . .
C57 C 0.60267(19) 0.2136(2) 0.14763(15) 0.0243(6) Uani 1 1 d . . .
H57 H 0.5916 0.18 0.1918 0.029 Uiso 1 1 calc R . .
C58 C 0.62169(18) 0.3247(2) 0.14768(14) 0.0194(5) Uani 1 1 d . . .
H58 H 0.6233 0.3677 0.1918 0.023 Uiso 1 1 calc R . .
C58A C 0.63895(18) 0.3760(2) 0.08251(13) 0.0179(5) Uani 1 1 d . . .
B1 B 0.5127(2) 0.9014(2) 0.19429(17) 0.0222(6) Uani 1 1 d . . .
F1 F 0.45670(12) 0.80575(12) 0.19977(8) 0.0320(4) Uani 1 1 d . . .
F2 F 0.58279(11) 0.87610(12) 0.15266(8) 0.0286(4) Uani 1 1 d . . .
F3 F 0.44027(13) 0.98105(13) 0.15561(9) 0.0427(4) Uani 1 1 d . . .
F4 F 0.57102(12) 0.93638(14) 0.26821(9) 0.0440(5) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N5 1.305(3) . ?
C1 N2 1.318(3) . ?
C1 H1 0.95 . ?
N2 C21 1.437(3) . ?
N2 C3 1.492(3) . ?
C3 C4 1.540(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.493(3) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.441(3) . ?
C21 C22 1.381(3) . ?
C21 C28A 1.419(3) . ?
C22 C23 1.429(3) . ?
C22 N221 1.436(3) . ?
N221 C226 1.460(3) . ?
N221 C122 1.477(3) . ?
C122 C223 1.511(3) . ?
C122 H22A 0.99 . ?
C122 H22B 0.99 . ?
C223 O224 1.426(3) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
O224 C225 1.428(3) . ?
C225 C226 1.517(3) . ?
C225 H22E 0.99 . ?
C225 H22F 0.99 . ?
C226 H22G 0.99 . ?
C226 H22H 0.99 . ?
C23 C24 1.360(3) . ?
C23 H23 0.95 . ?
C24 C24A 1.413(3) . ?
C24 H24 0.95 . ?
C24A C25 1.417(3) . ?
C24A C28A 1.432(3) . ?
C25 C26 1.371(3) . ?
C25 H25 0.95 . ?
C26 C27 1.412(3) . ?
C26 H26 0.95 . ?
C27 C28 1.377(3) . ?
C27 H27 0.95 . ?
C28 C28A 1.424(3) . ?
C28 H28 0.95 . ?
C51 C52 1.390(3) . ?
C51 C58A 1.432(3) . ?
C52 C53 1.411(3) . ?
C52 N521 1.424(3) . ?
N521 C526 1.469(3) . ?
N521 C522 1.476(3) . ?
C522 C523 1.513(3) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 O524 1.431(3) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
O524 C525 1.419(3) . ?
C525 C526 1.504(3) . ?
C525 H52E 0.99 . ?
C525 H52F 0.99 . ?
C526 H52G 0.99 . ?
C526 H52H 0.99 . ?
C53 C54 1.364(3) . ?
C53 H53 0.95 . ?
C54 C54A 1.414(3) . ?
C54 H54 0.95 . ?
C54A C58A 1.414(3) . ?
C54A C55 1.428(3) . ?
C55 C56 1.364(3) . ?
C55 H55 0.95 . ?
C56 C57 1.414(3) . ?
C56 H56 0.95 . ?
C57 C58 1.370(3) . ?
C57 H57 0.95 . ?
C58 C58A 1.417(3) . ?
C58 H58 0.95 . ?
B1 F3 1.383(3) . ?
B1 F4 1.383(3) . ?
B1 F1 1.396(3) . ?
B1 F2 1.401(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 C1 N2 115.0(2) . . ?
N5 C1 H1 122.5 . . ?
N2 C1 H1 122.5 . . ?
C1 N2 C21 119.69(19) . . ?
C1 N2 C3 107.95(18) . . ?
C21 N2 C3 124.42(18) . . ?
N2 C3 C4 101.95(17) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.2 . . ?
N5 C4 C3 101.86(17) . . ?
N5 C4 H4A 111.4 . . ?
C3 C4 H4A 111.4 . . ?
N5 C4 H4B 111.4 . . ?
C3 C4 H4B 111.4 . . ?
H4A C4 H4B 109.3 . . ?
C1 N5 C51 122.15(19) . . ?
C1 N5 C4 108.81(19) . . ?
C51 N5 C4 127.54(18) . . ?
C22 C21 C28A 122.4(2) . . ?
C22 C21 N2 118.0(2) . . ?
C28A C21 N2 119.6(2) . . ?
C21 C22 C23 118.7(2) . . ?
C21 C22 N221 118.4(2) . . ?
C23 C22 N221 122.8(2) . . ?
C22 N221 C226 114.85(18) . . ?
C22 N221 C122 110.67(17) . . ?
C226 N221 C122 110.07(18) . . ?
N221 C122 C223 108.43(18) . . ?
N221 C122 H22A 110 . . ?
C223 C122 H22A 110 . . ?
N221 C122 H22B 110 . . ?
C223 C122 H22B 110 . . ?
H22A C122 H22B 108.4 . . ?
O224 C223 C122 111.2(2) . . ?
O224 C223 H22C 109.4 . . ?
C122 C223 H22C 109.4 . . ?
O224 C223 H22D 109.4 . . ?
C122 C223 H22D 109.4 . . ?
H22C C223 H22D 108 . . ?
C223 O224 C225 110.31(18) . . ?
O224 C225 C226 111.38(19) . . ?
O224 C225 H22E 109.4 . . ?
C226 C225 H22E 109.4 . . ?
O224 C225 H22F 109.4 . . ?
C226 C225 H22F 109.4 . . ?
H22E C225 H22F 108 . . ?
N221 C226 C225 108.15(19) . . ?
N221 C226 H22G 110.1 . . ?
C225 C226 H22G 110.1 . . ?
N221 C226 H22H 110.1 . . ?
C225 C226 H22H 110.1 . . ?
H22G C226 H22H 108.4 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C24A 121.8(2) . . ?
C23 C24 H24 119.1 . . ?
C24A C24 H24 119.1 . . ?
C24 C24A C25 122.2(2) . . ?
C24 C24A C28A 119.1(2) . . ?
C25 C24A C28A 118.6(2) . . ?
C26 C25 C24A 120.7(2) . . ?
C26 C25 H25 119.7 . . ?
C24A C25 H25 119.7 . . ?
C25 C26 C27 120.9(2) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 120.1(2) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C28A 120.3(2) . . ?
C27 C28 H28 119.9 . . ?
C28A C28 H28 119.9 . . ?
C21 C28A C28 123.1(2) . . ?
C21 C28A C24A 117.6(2) . . ?
C28 C28A C24A 119.3(2) . . ?
C52 C51 C58A 122.0(2) . . ?
C52 C51 N5 119.6(2) . . ?
C58A C51 N5 117.9(2) . . ?
C51 C52 C53 117.9(2) . . ?
C51 C52 N521 120.1(2) . . ?
C53 C52 N521 121.8(2) . . ?
C52 N521 C526 116.22(18) . . ?
C52 N521 C522 116.67(19) . . ?
C526 N521 C522 108.19(18) . . ?
N521 C522 C523 109.7(2) . . ?
N521 C522 H52A 109.7 . . ?
C523 C522 H52A 109.7 . . ?
N521 C522 H52B 109.7 . . ?
C523 C522 H52B 109.7 . . ?
H52A C522 H52B 108.2 . . ?
O524 C523 C522 112.0(2) . . ?
O524 C523 H52C 109.2 . . ?
C522 C523 H52C 109.2 . . ?
O524 C523 H52D 109.2 . . ?
C522 C523 H52D 109.2 . . ?
H52C C523 H52D 107.9 . . ?
C525 O524 C523 110.69(18) . . ?
O524 C525 C526 112.1(2) . . ?
O524 C525 H52E 109.2 . . ?
C526 C525 H52E 109.2 . . ?
O524 C525 H52F 109.2 . . ?
C526 C525 H52F 109.2 . . ?
H52E C525 H52F 107.9 . . ?
N521 C526 C525 108.09(18) . . ?
N521 C526 H52G 110.1 . . ?
C525 C526 H52G 110.1 . . ?
N521 C526 H52H 110.1 . . ?
C525 C526 H52H 110.1 . . ?
H52G C526 H52H 108.4 . . ?
C54 C53 C52 121.4(2) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C53 C54 C54A 121.4(2) . . ?
C53 C54 H54 119.3 . . ?
C54A C54 H54 119.3 . . ?
C54 C54A C58A 119.0(2) . . ?
C54 C54A C55 121.7(2) . . ?
C58A C54A C55 119.3(2) . . ?
C56 C55 C54A 120.1(2) . . ?
C56 C55 H55 120 . . ?
C54A C55 H55 120 . . ?
C55 C56 C57 120.7(2) . . ?
C55 C56 H56 119.7 . . ?
C57 C56 H56 119.7 . . ?
C58 C57 C56 120.3(2) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C58A 120.6(2) . . ?
C57 C58 H58 119.7 . . ?
C58A C58 H58 119.7 . . ?
C54A C58A C58 119.0(2) . . ?
C54A C58A C51 118.1(2) . . ?
C58 C58A C51 122.8(2) . . ?
F3 B1 F4 111.1(2) . . ?
F3 B1 F1 108.7(2) . . ?
F4 B1 F1 109.2(2) . . ?
F3 B1 F2 110.4(2) . . ?
F4 B1 F2 109.3(2) . . ?
F1 B1 F2 108.1(2) . . ?

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

data_rda091
_database_code_depnum_ccdc_archive 'CCDC 1518957'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2012-10-16T15:34:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C33 H37 B F4 N4'
_chemical_formula_moiety         'C33 H37 N4, B F4'
_chemical_formula_weight         576.48

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-p 2ybc'
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                   13.5331(2)
_cell_length_b                   12.1105(2)
_cell_length_c                   18.6051(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.562(2)
_cell_angle_gamma                90
_cell_volume                     2873.23(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8954
_cell_measurement_theta_min      2.8179
_cell_measurement_theta_max      29.8823

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

_exptl_crystal_description       slab
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  CrysAlisPro, Agilent Technologies,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.98867
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      0.0154815
_diffrn_orient_matrix_ub_12      0.0257496
_diffrn_orient_matrix_ub_13      -0.0287997
_diffrn_orient_matrix_ub_21      -0.0024888
_diffrn_orient_matrix_ub_22      0.0524158
_diffrn_orient_matrix_ub_23      0.0163623
_diffrn_orient_matrix_ub_31      0.0533532
_diffrn_orient_matrix_ub_32      -0.0049613
_diffrn_orient_matrix_ub_33      0.0231677
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_number            23843
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         28.5
_diffrn_reflns_theta_full        28.5
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             7254
_reflns_number_gt                6074
_reflns_threshold_expression     >2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

The tetrafluoroborate anion was modelled as being disordered over two sets of
site with occupancies refined to 0.715(5) and its complement. The F atoms
of the minor component were refined with isotropic displacement parameters.
Geometries of the minor component were restrained to ideal values.

;
_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)+(0.0368P)²+1.3634P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7254
_refine_ls_number_parameters     392
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.044

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.27910(10) 0.44423(11) 0.45089(8) 0.0141(3) Uani 1 1 d . . .
H1 H 0.338 0.4597 0.4948 0.017 Uiso 1 1 calc R . .
N2 N 0.28578(9) 0.38411(10) 0.39370(6) 0.0140(2) Uani 1 1 d . . .
C21 C 0.38597(10) 0.36444(12) 0.38536(7) 0.0140(3) Uani 1 1 d . . .
C22 C 0.44210(10) 0.45303(11) 0.37341(7) 0.0147(3) Uani 1 1 d . . .
N221 N 0.39370(9) 0.55979(10) 0.36148(6) 0.0154(2) Uani 1 1 d . . .
C222 C 0.36988(12) 0.59516(12) 0.28160(8) 0.0196(3) Uani 1 1 d . . .
H22A H 0.3318 0.5356 0.2469 0.024 Uiso 1 1 calc R . .
H22B H 0.436 0.6096 0.2715 0.024 Uiso 1 1 calc R . .
C223 C 0.30346(12) 0.69890(13) 0.26653(9) 0.0235(3) Uani 1 1 d . . .
H22C H 0.2355 0.683 0.2735 0.028 Uiso 1 1 calc R . .
H22D H 0.2891 0.7229 0.2131 0.028 Uiso 1 1 calc R . .
C224 C 0.35934(13) 0.79131(13) 0.32059(9) 0.0254(3) Uani 1 1 d . . .
H22E H 0.3121 0.8558 0.3135 0.03 Uiso 1 1 calc R . .
H22F H 0.4223 0.8146 0.3087 0.03 Uiso 1 1 calc R . .
C225 C 0.39182(12) 0.75203(12) 0.40330(9) 0.0222(3) Uani 1 1 d . . .
H22G H 0.435 0.8097 0.4372 0.027 Uiso 1 1 calc R . .
H22H H 0.3284 0.7405 0.4176 0.027 Uiso 1 1 calc R . .
C226 C 0.45400(11) 0.64492(12) 0.41471(8) 0.0178(3) Uani 1 1 d . . .
H22I H 0.5213 0.6581 0.406 0.021 Uiso 1 1 calc R . .
H22J H 0.4699 0.6189 0.4678 0.021 Uiso 1 1 calc R . .
C23 C 0.54492(11) 0.43482(12) 0.37163(8) 0.0173(3) Uani 1 1 d . . .
H23 H 0.5846 0.4953 0.3634 0.021 Uiso 1 1 calc R . .
C24 C 0.58736(11) 0.33117(13) 0.38159(8) 0.0186(3) Uani 1 1 d . . .
H24 H 0.6572 0.3211 0.3821 0.022 Uiso 1 1 calc R . .
C24A C 0.52916(11) 0.23852(12) 0.39124(8) 0.0175(3) Uani 1 1 d . . .
C25 C 0.57061(12) 0.13003(13) 0.39973(9) 0.0229(3) Uani 1 1 d . . .
H25 H 0.6401 0.1182 0.4 0.027 Uiso 1 1 calc R . .
C26 C 0.51178(13) 0.04222(13) 0.40759(10) 0.0279(4) Uani 1 1 d . . .
H26 H 0.5403 -0.0302 0.4127 0.033 Uiso 1 1 calc R . .
C27 C 0.40854(13) 0.05857(13) 0.40812(10) 0.0265(3) Uani 1 1 d . . .
H27 H 0.3682 -0.0032 0.4135 0.032 Uiso 1 1 calc R . .
C28 C 0.36595(12) 0.16216(12) 0.40104(8) 0.0205(3) Uani 1 1 d . . .
H28 H 0.2967 0.172 0.4018 0.025 Uiso 1 1 calc R . .
C28A C 0.42523(11) 0.25482(12) 0.39258(8) 0.0160(3) Uani 1 1 d . . .
C3 C 0.18479(10) 0.39361(13) 0.32906(8) 0.0180(3) Uani 1 1 d . . .
H3A H 0.1613 0.3209 0.3051 0.022 Uiso 1 1 calc R . .
H3B H 0.1908 0.4459 0.2898 0.022 Uiso 1 1 calc R . .
C4 C 0.11027(11) 0.43783(13) 0.36908(8) 0.0184(3) Uani 1 1 d . . .
H4A H 0.0649 0.4974 0.3391 0.022 Uiso 1 1 calc R . .
H4B H 0.0657 0.3783 0.3781 0.022 Uiso 1 1 calc R . .
N5 N 0.18519(9) 0.48084(10) 0.44244(6) 0.0153(2) Uani 1 1 d . . .
C51 C 0.16139(10) 0.54028(12) 0.50170(8) 0.0162(3) Uani 1 1 d . . .
C52 C 0.17679(10) 0.49077(12) 0.57207(8) 0.0172(3) Uani 1 1 d . . .
N521 N 0.21843(9) 0.38266(10) 0.58853(7) 0.0176(3) Uani 1 1 d . . .
C522 C 0.25952(12) 0.35266(14) 0.67025(8) 0.0242(3) Uani 1 1 d . . .
H52A H 0.2005 0.343 0.6898 0.029 Uiso 1 1 calc R . .
H52B H 0.3048 0.4129 0.6996 0.029 Uiso 1 1 calc R . .
C523 C 0.32240(13) 0.24628(15) 0.68106(9) 0.0291(4) Uani 1 1 d . . .
H52C H 0.3477 0.2262 0.7358 0.035 Uiso 1 1 calc R . .
H52D H 0.3844 0.2582 0.6651 0.035 Uiso 1 1 calc R . .
C524 C 0.25742(13) 0.15177(14) 0.63507(9) 0.0286(4) Uani 1 1 d . . .
H52E H 0.201 0.1323 0.6556 0.034 Uiso 1 1 calc R . .
H52F H 0.3024 0.086 0.6392 0.034 Uiso 1 1 calc R . .
C525 C 0.20972(14) 0.18600(14) 0.55184(9) 0.0280(4) Uani 1 1 d . . .
H52G H 0.2661 0.1959 0.5295 0.034 Uiso 1 1 calc R . .
H52H H 0.1621 0.1272 0.5229 0.034 Uiso 1 1 calc R . .
C526 C 0.14917(11) 0.29306(12) 0.54543(8) 0.0212(3) Uani 1 1 d . . .
H52I H 0.1187 0.3144 0.4911 0.025 Uiso 1 1 calc R . .
H52J H 0.0909 0.2821 0.5656 0.025 Uiso 1 1 calc R . .
C53 C 0.15510(11) 0.55607(13) 0.62864(8) 0.0206(3) Uani 1 1 d . . .
H53 H 0.1611 0.5235 0.6764 0.025 Uiso 1 1 calc R . .
C54 C 0.12584(11) 0.66435(13) 0.61610(9) 0.0216(3) Uani 1 1 d . . .
H54 H 0.1114 0.7049 0.6552 0.026 Uiso 1 1 calc R . .
C54A C 0.11647(11) 0.71743(13) 0.54650(9) 0.0204(3) Uani 1 1 d . . .
C55 C 0.09274(11) 0.83167(13) 0.53454(10) 0.0256(3) Uani 1 1 d . . .
H55 H 0.0827 0.8747 0.5743 0.031 Uiso 1 1 calc R . .
C56 C 0.08419(12) 0.88006(14) 0.46659(10) 0.0292(4) Uani 1 1 d . . .
H56 H 0.0687 0.9566 0.4593 0.035 Uiso 1 1 calc R . .
C57 C 0.09830(12) 0.81702(14) 0.40719(10) 0.0275(3) Uani 1 1 d . . .
H57 H 0.0912 0.8513 0.3598 0.033 Uiso 1 1 calc R . .
C58 C 0.12212(11) 0.70670(13) 0.41685(9) 0.0222(3) Uani 1 1 d . . .
H58 H 0.1319 0.6656 0.3763 0.027 Uiso 1 1 calc R . .
C58A C 0.13222(10) 0.65344(12) 0.48697(8) 0.0182(3) Uani 1 1 d . . .
B1 B 0.03962(16) 0.11399(17) 0.30539(10) 0.0299(4) Uani 1 1 d D . .
F1 F 0.09655(8) 0.15370(10) 0.37640(5) 0.0383(3) Uani 1 1 d D A .
F2 F -0.01027(16) 0.21074(15) 0.26476(10) 0.0488(8) Uani 0.715(5) 1 d P A 1
F3 F -0.0446(2) 0.0499(3) 0.3095(2) 0.0328(7) Uani 0.715(5) 1 d P A 1
F4 F 0.09194(18) 0.0603(2) 0.26889(16) 0.0580(8) Uani 0.715(5) 1 d P A 1
F5 F 0.0374(4) 0.1799(4) 0.2444(2) 0.0457(15) Uiso 0.285(5) 1 d PD A 2
F6 F -0.0442(8) 0.0572(12) 0.3030(8) 0.083(5) Uiso 0.285(5) 1 d PD A 2
F7 F 0.1230(4) 0.0322(4) 0.3012(4) 0.0506(16) Uiso 0.285(5) 1 d PD A 2



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N5 1.3049(17) . ?
C1 N2 1.3171(17) . ?
C1 H1 0.95 . ?
N2 C21 1.4354(17) . ?
N2 C3 1.4923(17) . ?
C21 C22 1.3750(19) . ?
C21 C28A 1.4195(19) . ?
C22 C23 1.4201(19) . ?
C22 N221 1.4326(18) . ?
N221 C226 1.4726(17) . ?
N221 C222 1.4749(17) . ?
C222 C223 1.515(2) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 C224 1.525(2) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
C224 C225 1.528(2) . ?
C224 H22E 0.99 . ?
C224 H22F 0.99 . ?
C225 C226 1.522(2) . ?
C225 H22G 0.99 . ?
C225 H22H 0.99 . ?
C226 H22I 0.99 . ?
C226 H22J 0.99 . ?
C23 C24 1.367(2) . ?
C23 H23 0.95 . ?
C24 C24A 1.416(2) . ?
C24 H24 0.95 . ?
C24A C25 1.417(2) . ?
C24A C28A 1.4288(19) . ?
C25 C26 1.365(2) . ?
C25 H25 0.95 . ?
C26 C27 1.414(2) . ?
C26 H26 0.95 . ?
C27 C28 1.368(2) . ?
C27 H27 0.95 . ?
C28 C28A 1.418(2) . ?
C28 H28 0.95 . ?
C3 C4 1.5366(19) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.4952(17) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.4405(17) . ?
C51 C52 1.391(2) . ?
C51 C58A 1.427(2) . ?
C52 N521 1.4176(19) . ?
C52 C53 1.424(2) . ?
N521 C522 1.4788(18) . ?
N521 C526 1.4818(18) . ?
C522 C523 1.520(2) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 C524 1.520(2) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
C524 C525 1.522(2) . ?
C524 H52E 0.99 . ?
C524 H52F 0.99 . ?
C525 C526 1.517(2) . ?
C525 H52G 0.99 . ?
C525 H52H 0.99 . ?
C526 H52I 0.99 . ?
C526 H52J 0.99 . ?
C53 C54 1.367(2) . ?
C53 H53 0.95 . ?
C54 C54A 1.413(2) . ?
C54 H54 0.95 . ?
C54A C55 1.421(2) . ?
C54A C58A 1.425(2) . ?
C55 C56 1.363(2) . ?
C55 H55 0.95 . ?
C56 C57 1.408(2) . ?
C56 H56 0.95 . ?
C57 C58 1.372(2) . ?
C57 H57 0.95 . ?
C58 C58A 1.420(2) . ?
C58 H58 0.95 . ?
B1 F4 1.307(3) . ?
B1 F6 1.314(8) . ?
B1 F1 1.374(2) . ?
B1 F5 1.380(4) . ?
B1 F3 1.403(3) . ?
B1 F2 1.435(3) . ?
B1 F7 1.523(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 C1 N2 114.71(12) . . ?
N5 C1 H1 122.6 . . ?
N2 C1 H1 122.6 . . ?
C1 N2 C21 120.13(11) . . ?
C1 N2 C3 108.44(11) . . ?
C21 N2 C3 124.69(11) . . ?
C22 C21 C28A 122.39(12) . . ?
C22 C21 N2 118.75(12) . . ?
C28A C21 N2 118.82(12) . . ?
C21 C22 C23 118.76(13) . . ?
C21 C22 N221 118.73(12) . . ?
C23 C22 N221 122.50(12) . . ?
C22 N221 C226 113.95(11) . . ?
C22 N221 C222 110.64(11) . . ?
C226 N221 C222 111.06(11) . . ?
N221 C222 C223 110.07(12) . . ?
N221 C222 H22A 109.6 . . ?
C223 C222 H22A 109.6 . . ?
N221 C222 H22B 109.6 . . ?
C223 C222 H22B 109.6 . . ?
H22A C222 H22B 108.2 . . ?
C222 C223 C224 110.72(12) . . ?
C222 C223 H22C 109.5 . . ?
C224 C223 H22C 109.5 . . ?
C222 C223 H22D 109.5 . . ?
C224 C223 H22D 109.5 . . ?
H22C C223 H22D 108.1 . . ?
C223 C224 C225 110.34(13) . . ?
C223 C224 H22E 109.6 . . ?
C225 C224 H22E 109.6 . . ?
C223 C224 H22F 109.6 . . ?
C225 C224 H22F 109.6 . . ?
H22E C224 H22F 108.1 . . ?
C226 C225 C224 111.41(13) . . ?
C226 C225 H22G 109.3 . . ?
C224 C225 H22G 109.3 . . ?
C226 C225 H22H 109.3 . . ?
C224 C225 H22H 109.3 . . ?
H22G C225 H22H 108 . . ?
N221 C226 C225 110.29(11) . . ?
N221 C226 H22I 109.6 . . ?
C225 C226 H22I 109.6 . . ?
N221 C226 H22J 109.6 . . ?
C225 C226 H22J 109.6 . . ?
H22I C226 H22J 108.1 . . ?
C24 C23 C22 120.66(13) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C24A 121.22(13) . . ?
C23 C24 H24 119.4 . . ?
C24A C24 H24 119.4 . . ?
C24 C24A C25 122.18(13) . . ?
C24 C24A C28A 119.03(13) . . ?
C25 C24A C28A 118.79(13) . . ?
C26 C25 C24A 120.73(14) . . ?
C26 C25 H25 119.6 . . ?
C24A C25 H25 119.6 . . ?
C25 C26 C27 120.30(14) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 120.86(15) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C28A 120.02(14) . . ?
C27 C28 H28 120 . . ?
C28A C28 H28 120 . . ?
C28 C28A C21 122.87(13) . . ?
C28 C28A C24A 119.29(13) . . ?
C21 C28A C24A 117.84(13) . . ?
N2 C3 C4 102.06(11) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.2 . . ?
N5 C4 C3 102.08(10) . . ?
N5 C4 H4A 111.4 . . ?
C3 C4 H4A 111.4 . . ?
N5 C4 H4B 111.4 . . ?
C3 C4 H4B 111.4 . . ?
H4A C4 H4B 109.2 . . ?
C1 N5 C51 122.41(11) . . ?
C1 N5 C4 109.08(11) . . ?
C51 N5 C4 128.00(11) . . ?
C52 C51 C58A 122.65(13) . . ?
C52 C51 N5 120.23(13) . . ?
C58A C51 N5 116.83(12) . . ?
C51 C52 N521 121.67(13) . . ?
C51 C52 C53 116.97(14) . . ?
N521 C52 C53 121.25(13) . . ?
C52 N521 C522 115.76(12) . . ?
C52 N521 C526 115.20(11) . . ?
C522 N521 C526 109.18(12) . . ?
N521 C522 C523 110.21(13) . . ?
N521 C522 H52A 109.6 . . ?
C523 C522 H52A 109.6 . . ?
N521 C522 H52B 109.6 . . ?
C523 C522 H52B 109.6 . . ?
H52A C522 H52B 108.1 . . ?
C522 C523 C524 111.78(13) . . ?
C522 C523 H52C 109.3 . . ?
C524 C523 H52C 109.3 . . ?
C522 C523 H52D 109.3 . . ?
C524 C523 H52D 109.3 . . ?
H52C C523 H52D 107.9 . . ?
C523 C524 C525 109.62(14) . . ?
C523 C524 H52E 109.7 . . ?
C525 C524 H52E 109.7 . . ?
C523 C524 H52F 109.7 . . ?
C525 C524 H52F 109.7 . . ?
H52E C524 H52F 108.2 . . ?
C526 C525 C524 110.28(13) . . ?
C526 C525 H52G 109.6 . . ?
C524 C525 H52G 109.6 . . ?
C526 C525 H52H 109.6 . . ?
C524 C525 H52H 109.6 . . ?
H52G C525 H52H 108.1 . . ?
N521 C526 C525 110.87(12) . . ?
N521 C526 H52I 109.5 . . ?
C525 C526 H52I 109.5 . . ?
N521 C526 H52J 109.5 . . ?
C525 C526 H52J 109.5 . . ?
H52I C526 H52J 108.1 . . ?
C54 C53 C52 121.76(14) . . ?
C54 C53 H53 119.1 . . ?
C52 C53 H53 119.1 . . ?
C53 C54 C54A 121.65(14) . . ?
C53 C54 H54 119.2 . . ?
C54A C54 H54 119.2 . . ?
C54 C54A C55 122.19(14) . . ?
C54 C54A C58A 118.30(14) . . ?
C55 C54A C58A 119.50(14) . . ?
C56 C55 C54A 120.57(15) . . ?
C56 C55 H55 119.7 . . ?
C54A C55 H55 119.7 . . ?
C55 C56 C57 120.23(15) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C58 C57 C56 120.85(16) . . ?
C58 C57 H57 119.6 . . ?
C56 C57 H57 119.6 . . ?
C57 C58 C58A 120.58(15) . . ?
C57 C58 H58 119.7 . . ?
C58A C58 H58 119.7 . . ?
C58 C58A C54A 118.27(14) . . ?
C58 C58A C51 123.22(13) . . ?
C54A C58A C51 118.47(13) . . ?
F4 B1 F1 116.54(19) . . ?
F6 B1 F1 114.5(6) . . ?
F6 B1 F5 119.6(7) . . ?
F1 B1 F5 116.0(2) . . ?
F4 B1 F3 110.2(2) . . ?
F1 B1 F3 110.20(19) . . ?
F4 B1 F2 112.0(2) . . ?
F1 B1 F2 103.54(15) . . ?
F3 B1 F2 103.5(2) . . ?
F6 B1 F7 107.7(7) . . ?
F1 B1 F7 95.2(3) . . ?
F5 B1 F7 98.4(3) . . ?


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

data_rda005
_database_code_depnum_ccdc_archive 'CCDC 1518958'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2012-08-05T21:18:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C31 H32 N4 O2'
_chemical_formula_moiety         'C31 H32 N4 O2'
_chemical_formula_weight         492.61

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-p 2ybc'

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                   24.3449(5)
_cell_length_b                   9.4072(2)
_cell_length_c                   22.6550(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.178(2)
_cell_angle_gamma                90
_cell_volume                     5180.41(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13668
_cell_measurement_theta_min      3.59
_cell_measurement_theta_max      30.0

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
   CrysAlisPro, Agilent Technologies,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.9416
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_number            53240
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.6
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_full        30
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             15095
_reflns_number_gt                11236
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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)+(0.0534P)²+2.7126P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         15095
_refine_ls_number_parameters     667
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.064
_refine_ls_wR_factor_ref         0.1449
_refine_ls_wR_factor_gt          0.1338
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.049

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.86825(6) 0.80052(16) 0.52244(7) 0.0219(3) Uani 1 1 d . . .
N2 N 0.91896(5) 0.85699(14) 0.53324(6) 0.0227(3) Uani 1 1 d . . .
C21 C 0.96886(6) 0.77922(16) 0.54352(8) 0.0254(3) Uani 1 1 d . . .
C22 C 0.99606(7) 0.78385(18) 0.59904(8) 0.0292(4) Uani 1 1 d . . .
N221 N 0.97185(6) 0.85643(16) 0.64541(6) 0.0300(3) Uani 1 1 d . . .
C222 C 1.00787(8) 0.9108(2) 0.69457(9) 0.0381(4) Uani 1 1 d . . .
H22A H 1.0405 0.9574 0.679 0.046 Uiso 1 1 calc R . .
H22B H 1.0206 0.8313 0.7205 0.046 Uiso 1 1 calc R . .
C223 C 0.97612(8) 1.0159(2) 0.72909(9) 0.0419(5) Uani 1 1 d . . .
H22C H 0.9999 1.0517 0.7627 0.05 Uiso 1 1 calc R . .
H22D H 0.9657 1.0978 0.7034 0.05 Uiso 1 1 calc R . .
O224 O 0.92790(6) 0.95540(16) 0.75099(6) 0.0435(3) Uani 1 1 d . . .
C225 C 0.89315(8) 0.8994(2) 0.70336(8) 0.0340(4) Uani 1 1 d . . .
H22E H 0.8806 0.9779 0.6768 0.041 Uiso 1 1 calc R . .
H22F H 0.8603 0.8552 0.7195 0.041 Uiso 1 1 calc R . .
C226 C 0.92299(7) 0.79007(18) 0.66838(8) 0.0287(3) Uani 1 1 d . . .
H22G H 0.9339 0.7086 0.694 0.034 Uiso 1 1 calc R . .
H22H H 0.8985 0.7545 0.6353 0.034 Uiso 1 1 calc R . .
C23 C 1.04846(7) 0.7182(2) 0.60716(9) 0.0351(4) Uani 1 1 d . . .
H23 H 1.0675 0.7211 0.6449 0.042 Uiso 1 1 calc R . .
C24 C 1.07150(7) 0.65152(19) 0.56176(9) 0.0372(4) Uani 1 1 d . . .
H24 H 1.1063 0.6071 0.5686 0.045 Uiso 1 1 calc R . .
C24A C 1.04549(7) 0.64589(18) 0.50453(9) 0.0332(4) Uani 1 1 d . . .
C25 C 1.06958(7) 0.58166(19) 0.45597(10) 0.0386(5) Uani 1 1 d . . .
H25 H 1.1038 0.5337 0.462 0.046 Uiso 1 1 calc R . .
C26 C 1.04498(8) 0.5870(2) 0.40118(10) 0.0418(5) Uani 1 1 d . . .
H26 H 1.0623 0.5441 0.3691 0.05 Uiso 1 1 calc R . .
C27 C 0.99333(8) 0.6563(2) 0.39097(9) 0.0385(4) Uani 1 1 d . . .
H27 H 0.9766 0.661 0.3521 0.046 Uiso 1 1 calc R . .
C28 C 0.96792(7) 0.71616(18) 0.43740(8) 0.0313(4) Uani 1 1 d . . .
H28 H 0.9331 0.7606 0.4306 0.038 Uiso 1 1 calc R . .
C28A C 0.99279(6) 0.71268(17) 0.49505(8) 0.0278(3) Uani 1 1 d . . .
C3 C 0.92314(6) 1.01168(17) 0.52179(8) 0.0256(3) Uani 1 1 d . . .
H3A H 0.9443 1.031 0.4866 0.031 Uiso 1 1 calc R . .
H3B H 0.9404 1.0624 0.5563 0.031 Uiso 1 1 calc R . .
C4 C 0.86284(6) 1.05302(17) 0.51110(8) 0.0280(3) Uani 1 1 d . . .
H4A H 0.8497 1.1101 0.5442 0.034 Uiso 1 1 calc R . .
H4B H 0.8566 1.1068 0.4737 0.034 Uiso 1 1 calc R . .
N5 N 0.83580(5) 0.91195(13) 0.50762(6) 0.0208(3) Uani 1 1 d . . .
C51 C 0.77729(6) 0.91104(16) 0.49857(7) 0.0218(3) Uani 1 1 d . . .
C52 C 0.75351(6) 0.92633(16) 0.44169(7) 0.0241(3) Uani 1 1 d . . .
N521 N 0.78731(6) 0.91871(14) 0.39281(6) 0.0260(3) Uani 1 1 d . . .
C522 C 0.76375(8) 0.9743(2) 0.33666(8) 0.0347(4) Uani 1 1 d . . .
H52A H 0.7501 1.0722 0.3423 0.042 Uiso 1 1 calc R . .
H52B H 0.7323 0.9144 0.3225 0.042 Uiso 1 1 calc R . .
C523 C 0.80715(9) 0.9743(2) 0.29161(8) 0.0407(5) Uani 1 1 d . . .
H52C H 0.7912 1.0127 0.2537 0.049 Uiso 1 1 calc R . .
H52D H 0.8378 1.0374 0.3054 0.049 Uiso 1 1 calc R . .
O524 O 0.82801(7) 0.83507(15) 0.28212(6) 0.0455(4) Uani 1 1 d . . .
C525 C 0.85132(8) 0.7808(2) 0.33682(8) 0.0369(4) Uani 1 1 d . . .
H52E H 0.8823 0.8422 0.351 0.044 Uiso 1 1 calc R . .
H52F H 0.8659 0.6841 0.3305 0.044 Uiso 1 1 calc R . .
C526 C 0.80914(7) 0.77519(17) 0.38298(7) 0.0281(3) Uani 1 1 d . . .
H52G H 0.7788 0.7108 0.3697 0.034 Uiso 1 1 calc R . .
H52H H 0.8262 0.7375 0.4204 0.034 Uiso 1 1 calc R . .
C53 C 0.69605(7) 0.95089(19) 0.43485(8) 0.0312(4) Uani 1 1 d . . .
H53 H 0.6793 0.9635 0.3963 0.037 Uiso 1 1 calc R . .
C54 C 0.66434(7) 0.95678(19) 0.48257(9) 0.0333(4) Uani 1 1 d . . .
H54 H 0.6261 0.9764 0.4766 0.04 Uiso 1 1 calc R . .
C54A C 0.68677(7) 0.93458(17) 0.54033(8) 0.0295(4) Uani 1 1 d . . .
C55 C 0.65495(7) 0.9410(2) 0.59062(9) 0.0393(5) Uani 1 1 d . . .
H55 H 0.6165 0.9575 0.5857 0.047 Uiso 1 1 calc R . .
C56 C 0.67848(8) 0.9240(2) 0.64577(10) 0.0439(5) Uani 1 1 d . . .
H56 H 0.6563 0.9293 0.6789 0.053 Uiso 1 1 calc R . .
C57 C 0.73547(8) 0.8984(2) 0.65463(9) 0.0399(5) Uani 1 1 d . . .
H57 H 0.7514 0.8854 0.6935 0.048 Uiso 1 1 calc R . .
C58 C 0.76781(7) 0.89252(19) 0.60683(8) 0.0307(4) Uani 1 1 d . . .
H58 H 0.8062 0.8756 0.6129 0.037 Uiso 1 1 calc R . .
C58A C 0.74468(6) 0.91124(16) 0.54867(7) 0.0244(3) Uani 1 1 d . . .
C6 C 0.38336(6) 0.71949(16) 0.31779(6) 0.0196(3) Uani 1 1 d . . .
N7 N 0.33517(5) 0.64841(13) 0.31631(5) 0.0191(2) Uani 1 1 d . . .
C71 C 0.28118(6) 0.70732(16) 0.31231(6) 0.0192(3) Uani 1 1 d . . .
C72 C 0.24564(6) 0.67565(16) 0.35623(6) 0.0205(3) Uani 1 1 d . . .
N721 N 0.26750(5) 0.60927(14) 0.40865(5) 0.0209(3) Uani 1 1 d . . .
C722 C 0.22946(7) 0.53172(19) 0.44437(7) 0.0289(3) Uani 1 1 d . . .
H72A H 0.2068 0.4659 0.4191 0.035 Uiso 1 1 calc R . .
H72B H 0.2045 0.5991 0.4632 0.035 Uiso 1 1 calc R . .
C723 C 0.26251(8) 0.44911(19) 0.49117(8) 0.0327(4) Uani 1 1 d . . .
H72C H 0.2371 0.3953 0.5155 0.039 Uiso 1 1 calc R . .
H72D H 0.2863 0.3799 0.4718 0.039 Uiso 1 1 calc R . .
O724 O 0.29569(6) 0.53999(13) 0.52826(5) 0.0339(3) Uani 1 1 d . . .
C725 C 0.33265(8) 0.61875(19) 0.49375(7) 0.0310(4) Uani 1 1 d . . .
H72E H 0.3581 0.5522 0.4752 0.037 Uiso 1 1 calc R . .
H72F H 0.3549 0.6835 0.5199 0.037 Uiso 1 1 calc R . .
C726 C 0.30192(7) 0.70422(17) 0.44634(7) 0.0243(3) Uani 1 1 d . . .
H72G H 0.2786 0.776 0.4647 0.029 Uiso 1 1 calc R . .
H72H H 0.3284 0.7547 0.4221 0.029 Uiso 1 1 calc R . .
C73 C 0.18906(6) 0.70732(17) 0.34695(7) 0.0246(3) Uani 1 1 d . . .
H73 H 0.1645 0.6841 0.3766 0.03 Uiso 1 1 calc R . .
C74 C 0.16931(7) 0.77089(18) 0.29591(7) 0.0272(3) Uani 1 1 d . . .
H74 H 0.1309 0.7881 0.29 0.033 Uiso 1 1 calc R . .
C74A C 0.20491(7) 0.81145(17) 0.25170(7) 0.0249(3) Uani 1 1 d . . .
C75 C 0.18507(7) 0.87603(18) 0.19800(8) 0.0313(4) Uani 1 1 d . . .
H75 H 0.1471 0.8984 0.1923 0.038 Uiso 1 1 calc R . .
C76 C 0.21990(8) 0.90633(19) 0.15456(8) 0.0337(4) Uani 1 1 d . . .
H76 H 0.2058 0.9469 0.1184 0.04 Uiso 1 1 calc R . .
C77 C 0.27650(7) 0.87787(19) 0.16301(7) 0.0302(4) Uani 1 1 d . . .
H77 H 0.3006 0.901 0.1328 0.036 Uiso 1 1 calc R . .
C78 C 0.29713(7) 0.81700(17) 0.21445(7) 0.0251(3) Uani 1 1 d . . .
H78 H 0.3355 0.799 0.2197 0.03 Uiso 1 1 calc R . .
C78A C 0.26191(6) 0.78032(16) 0.26004(6) 0.0214(3) Uani 1 1 d . . .
C8 C 0.33967(6) 0.49266(17) 0.30688(7) 0.0258(3) Uani 1 1 d . . .
H8A H 0.3245 0.4648 0.2671 0.031 Uiso 1 1 calc R . .
H8B H 0.3206 0.4387 0.3372 0.031 Uiso 1 1 calc R . .
C9 C 0.40163(6) 0.47013(17) 0.31316(8) 0.0255(3) Uani 1 1 d . . .
H9A H 0.4127 0.4202 0.3504 0.031 Uiso 1 1 calc R . .
H9B H 0.415 0.416 0.2793 0.031 Uiso 1 1 calc R . .
N10 N 0.42196(5) 0.61833(13) 0.31364(5) 0.0203(3) Uani 1 1 d . . .
C101 C 0.48012(6) 0.63851(16) 0.32024(7) 0.0205(3) Uani 1 1 d . . .
C102 C 0.51143(6) 0.62697(16) 0.27113(7) 0.0230(3) Uani 1 1 d . . .
N111 N 0.48424(6) 0.61487(14) 0.21452(6) 0.0246(3) Uani 1 1 d . . .
C112 C 0.51551(8) 0.55615(19) 0.16665(8) 0.0323(4) Uani 1 1 d . . .
H11A H 0.5351 0.4688 0.1802 0.039 Uiso 1 1 calc R . .
H11B H 0.5431 0.6261 0.1545 0.039 Uiso 1 1 calc R . .
C113 C 0.47571(9) 0.5224(2) 0.11528(8) 0.0383(4) Uani 1 1 d . . .
H11C H 0.4962 0.482 0.0826 0.046 Uiso 1 1 calc R . .
H11D H 0.4492 0.4497 0.1276 0.046 Uiso 1 1 calc R . .
O114 O 0.44622(6) 0.64570(14) 0.09453(5) 0.0379(3) Uani 1 1 d . . .
C115 C 0.41718(7) 0.7078(2) 0.14100(7) 0.0305(4) Uani 1 1 d . . .
H11E H 0.3888 0.6404 0.1535 0.037 Uiso 1 1 calc R . .
H11F H 0.3983 0.7951 0.1263 0.037 Uiso 1 1 calc R . .
C116 C 0.45557(7) 0.74428(17) 0.19344(7) 0.0233(3) Uani 1 1 d . . .
H11G H 0.4827 0.816 0.1819 0.028 Uiso 1 1 calc R . .
H11H H 0.4344 0.7849 0.2255 0.028 Uiso 1 1 calc R . .
C103 C 0.56966(7) 0.62384(18) 0.27988(8) 0.0292(4) Uani 1 1 d . . .
H103 H 0.5916 0.6154 0.2466 0.035 Uiso 1 1 calc R . .
C104 C 0.59466(7) 0.63267(18) 0.33494(8) 0.0307(4) Uani 1 1 d . . .
H104 H 0.6336 0.6277 0.3395 0.037 Uiso 1 1 calc R . .
C10A C 0.56388(7) 0.64904(17) 0.38559(8) 0.0265(3) Uani 1 1 d . . .
C105 C 0.58892(8) 0.66286(19) 0.44322(8) 0.0341(4) Uani 1 1 d . . .
H105 H 0.6279 0.6601 0.4487 0.041 Uiso 1 1 calc R . .
C106 C 0.55799(8) 0.6800(2) 0.49083(8) 0.0369(4) Uani 1 1 d . . .
H106 H 0.5755 0.69 0.5291 0.044 Uiso 1 1 calc R . .
C107 C 0.50017(8) 0.6831(2) 0.48382(8) 0.0331(4) Uani 1 1 d . . .
H107 H 0.4789 0.6948 0.5174 0.04 Uiso 1 1 calc R . .
C108 C 0.47442(7) 0.66924(18) 0.42879(7) 0.0270(3) Uani 1 1 d . . .
H108 H 0.4354 0.6706 0.4246 0.032 Uiso 1 1 calc R . .
C10B C 0.50530(6) 0.65296(16) 0.37818(7) 0.0227(3) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N5 1.3440(19) . ?
C1 N2 1.3538(19) . ?
N2 C21 1.4261(19) . ?
N2 C3 1.483(2) . ?
C21 C22 1.389(2) . ?
C21 C28A 1.417(2) . ?
C22 N221 1.409(2) . ?
C22 C23 1.420(2) . ?
N221 C226 1.464(2) . ?
N221 C222 1.470(2) . ?
C222 C223 1.501(3) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 O224 1.419(2) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
O224 C225 1.434(2) . ?
C225 C226 1.509(3) . ?
C225 H22E 0.99 . ?
C225 H22F 0.99 . ?
C226 H22G 0.99 . ?
C226 H22H 0.99 . ?
C23 C24 1.353(3) . ?
C23 H23 0.95 . ?
C24 C24A 1.412(3) . ?
C24 H24 0.95 . ?
C24A C25 1.411(3) . ?
C24A C28A 1.434(2) . ?
C25 C26 1.349(3) . ?
C25 H25 0.95 . ?
C26 C27 1.424(3) . ?
C26 H26 0.95 . ?
C27 C28 1.371(2) . ?
C27 H27 0.95 . ?
C28 C28A 1.409(3) . ?
C28 H28 0.95 . ?
C3 C4 1.525(2) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.482(2) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.4278(18) . ?
C51 C52 1.391(2) . ?
C51 C58A 1.421(2) . ?
C52 N521 1.418(2) . ?
C52 C53 1.418(2) . ?
N521 C522 1.463(2) . ?
N521 C526 1.472(2) . ?
C522 C523 1.509(3) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 O524 1.426(2) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
O524 C525 1.428(2) . ?
C525 C526 1.506(2) . ?
C525 H52E 0.99 . ?
C525 H52F 0.99 . ?
C526 H52G 0.99 . ?
C526 H52H 0.99 . ?
C53 C54 1.364(3) . ?
C53 H53 0.95 . ?
C54 C54A 1.405(3) . ?
C54 H54 0.95 . ?
C54A C55 1.414(2) . ?
C54A C58A 1.429(2) . ?
C55 C56 1.355(3) . ?
C55 H55 0.95 . ?
C56 C57 1.412(3) . ?
C56 H56 0.95 . ?
C57 C58 1.375(2) . ?
C57 H57 0.95 . ?
C58 C58A 1.415(2) . ?
C58 H58 0.95 . ?
C6 N10 1.3443(19) . ?
C6 N7 1.3493(19) . ?
N7 C71 1.4247(18) . ?
N7 C8 1.486(2) . ?
C71 C72 1.387(2) . ?
C71 C78A 1.426(2) . ?
C72 C73 1.414(2) . ?
C72 N721 1.4187(19) . ?
N721 C722 1.4586(19) . ?
N721 C726 1.466(2) . ?
C722 C723 1.510(2) . ?
C722 H72A 0.99 . ?
C722 H72B 0.99 . ?
C723 O724 1.419(2) . ?
C723 H72C 0.99 . ?
C723 H72D 0.99 . ?
O724 C725 1.431(2) . ?
C725 C726 1.507(2) . ?
C725 H72E 0.99 . ?
C725 H72F 0.99 . ?
C726 H72G 0.99 . ?
C726 H72H 0.99 . ?
C73 C74 1.365(2) . ?
C73 H73 0.95 . ?
C74 C74A 1.413(2) . ?
C74 H74 0.95 . ?
C74A C75 1.420(2) . ?
C74A C78A 1.421(2) . ?
C75 C76 1.364(3) . ?
C75 H75 0.95 . ?
C76 C77 1.406(3) . ?
C76 H76 0.95 . ?
C77 C78 1.369(2) . ?
C77 H77 0.95 . ?
C78 C78A 1.421(2) . ?
C78 H78 0.95 . ?
C8 C9 1.522(2) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 N10 1.479(2) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
N10 C101 1.4280(18) . ?
C101 C102 1.387(2) . ?
C101 C10B 1.424(2) . ?
C102 N111 1.415(2) . ?
C102 C103 1.421(2) . ?
N111 C112 1.467(2) . ?
N111 C116 1.470(2) . ?
C112 C113 1.506(3) . ?
C112 H11A 0.99 . ?
C112 H11B 0.99 . ?
C113 O114 1.430(2) . ?
C113 H11C 0.99 . ?
C113 H11D 0.99 . ?
O114 C115 1.425(2) . ?
C115 C116 1.510(2) . ?
C115 H11E 0.99 . ?
C115 H11F 0.99 . ?
C116 H11G 0.99 . ?
C116 H11H 0.99 . ?
C103 C104 1.360(3) . ?
C103 H103 0.95 . ?
C104 C10A 1.413(2) . ?
C104 H104 0.95 . ?
C10A C105 1.416(2) . ?
C10A C10B 1.427(2) . ?
C105 C106 1.359(3) . ?
C105 H105 0.95 . ?
C106 C107 1.408(3) . ?
C106 H106 0.95 . ?
C107 C108 1.370(2) . ?
C107 H107 0.95 . ?
C108 C10B 1.414(2) . ?
C108 H108 0.95 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 C1 N2 104.87(13) . . ?
C1 N2 C21 126.03(13) . . ?
C1 N2 C3 115.10(12) . . ?
C21 N2 C3 117.78(12) . . ?
C22 C21 C28A 121.31(15) . . ?
C22 C21 N2 119.38(15) . . ?
C28A C21 N2 118.89(15) . . ?
C21 C22 N221 119.48(15) . . ?
C21 C22 C23 118.90(17) . . ?
N221 C22 C23 121.60(16) . . ?
C22 N221 C226 116.10(14) . . ?
C22 N221 C222 118.47(14) . . ?
C226 N221 C222 109.95(14) . . ?
N221 C222 C223 108.72(15) . . ?
N221 C222 H22A 109.9 . . ?
C223 C222 H22A 109.9 . . ?
N221 C222 H22B 109.9 . . ?
C223 C222 H22B 109.9 . . ?
H22A C222 H22B 108.3 . . ?
O224 C223 C222 112.19(17) . . ?
O224 C223 H22C 109.2 . . ?
C222 C223 H22C 109.2 . . ?
O224 C223 H22D 109.2 . . ?
C222 C223 H22D 109.2 . . ?
H22C C223 H22D 107.9 . . ?
C223 O224 C225 110.44(14) . . ?
O224 C225 C226 111.39(15) . . ?
O224 C225 H22E 109.3 . . ?
C226 C225 H22E 109.3 . . ?
O224 C225 H22F 109.3 . . ?
C226 C225 H22F 109.3 . . ?
H22E C225 H22F 108 . . ?
N221 C226 C225 108.69(14) . . ?
N221 C226 H22G 110 . . ?
C225 C226 H22G 110 . . ?
N221 C226 H22H 110 . . ?
C225 C226 H22H 110 . . ?
H22G C226 H22H 108.3 . . ?
C24 C23 C22 120.70(18) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C24A 122.13(16) . . ?
C23 C24 H24 118.9 . . ?
C24A C24 H24 118.9 . . ?
C25 C24A C24 123.19(17) . . ?
C25 C24A C28A 118.55(18) . . ?
C24 C24A C28A 118.23(17) . . ?
C26 C25 C24A 121.27(18) . . ?
C26 C25 H25 119.4 . . ?
C24A C25 H25 119.4 . . ?
C25 C26 C27 120.64(18) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C28 C27 C26 119.7(2) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C28A 120.85(17) . . ?
C27 C28 H28 119.6 . . ?
C28A C28 H28 119.6 . . ?
C28 C28A C21 122.28(15) . . ?
C28 C28A C24A 118.94(16) . . ?
C21 C28A C24A 118.71(16) . . ?
N2 C3 C4 101.73(12) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.3 . . ?
N5 C4 C3 101.60(12) . . ?
N5 C4 H4A 111.5 . . ?
C3 C4 H4A 111.5 . . ?
N5 C4 H4B 111.5 . . ?
C3 C4 H4B 111.5 . . ?
H4A C4 H4B 109.3 . . ?
C1 N5 C51 126.81(13) . . ?
C1 N5 C4 115.59(12) . . ?
C51 N5 C4 116.73(12) . . ?
C52 C51 C58A 121.19(14) . . ?
C52 C51 N5 119.55(13) . . ?
C58A C51 N5 118.84(14) . . ?
C51 C52 N521 119.26(14) . . ?
C51 C52 C53 118.41(15) . . ?
N521 C52 C53 122.32(15) . . ?
C52 N521 C522 116.40(13) . . ?
C52 N521 C526 113.25(13) . . ?
C522 N521 C526 108.87(13) . . ?
N521 C522 C523 109.44(15) . . ?
N521 C522 H52A 109.8 . . ?
C523 C522 H52A 109.8 . . ?
N521 C522 H52B 109.8 . . ?
C523 C522 H52B 109.8 . . ?
H52A C522 H52B 108.2 . . ?
O524 C523 C522 111.72(15) . . ?
O524 C523 H52C 109.3 . . ?
C522 C523 H52C 109.3 . . ?
O524 C523 H52D 109.3 . . ?
C522 C523 H52D 109.3 . . ?
H52C C523 H52D 107.9 . . ?
C523 O524 C525 108.98(14) . . ?
O524 C525 C526 111.19(16) . . ?
O524 C525 H52E 109.4 . . ?
C526 C525 H52E 109.4 . . ?
O524 C525 H52F 109.4 . . ?
C526 C525 H52F 109.4 . . ?
H52E C525 H52F 108 . . ?
N521 C526 C525 109.80(14) . . ?
N521 C526 H52G 109.7 . . ?
C525 C526 H52G 109.7 . . ?
N521 C526 H52H 109.7 . . ?
C525 C526 H52H 109.7 . . ?
H52G C526 H52H 108.2 . . ?
C54 C53 C52 121.22(16) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C53 C54 C54A 121.62(16) . . ?
C53 C54 H54 119.2 . . ?
C54A C54 H54 119.2 . . ?
C54 C54A C55 122.82(16) . . ?
C54 C54A C58A 118.40(15) . . ?
C55 C54A C58A 118.72(17) . . ?
C56 C55 C54A 121.04(17) . . ?
C56 C55 H55 119.5 . . ?
C54A C55 H55 119.5 . . ?
C55 C56 C57 120.88(17) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
C58 C57 C56 119.75(19) . . ?
C58 C57 H57 120.1 . . ?
C56 C57 H57 120.1 . . ?
C57 C58 C58A 120.85(17) . . ?
C57 C58 H58 119.6 . . ?
C58A C58 H58 119.6 . . ?
C58 C58A C51 122.19(15) . . ?
C58 C58A C54A 118.75(15) . . ?
C51 C58A C54A 119.04(15) . . ?
N10 C6 N7 104.94(13) . . ?
C6 N7 C71 127.36(13) . . ?
C6 N7 C8 114.92(12) . . ?
C71 N7 C8 116.72(12) . . ?
C72 C71 N7 118.75(13) . . ?
C72 C71 C78A 120.66(14) . . ?
N7 C71 C78A 120.01(13) . . ?
C71 C72 C73 119.31(14) . . ?
C71 C72 N721 118.37(13) . . ?
C73 C72 N721 122.31(13) . . ?
C72 N721 C722 117.67(13) . . ?
C72 N721 C726 113.27(12) . . ?
C722 N721 C726 109.97(12) . . ?
N721 C722 C723 108.49(14) . . ?
N721 C722 H72A 110 . . ?
C723 C722 H72A 110 . . ?
N721 C722 H72B 110 . . ?
C723 C722 H72B 110 . . ?
H72A C722 H72B 108.4 . . ?
O724 C723 C722 111.67(14) . . ?
O724 C723 H72C 109.3 . . ?
C722 C723 H72C 109.3 . . ?
O724 C723 H72D 109.3 . . ?
C722 C723 H72D 109.3 . . ?
H72C C723 H72D 107.9 . . ?
C723 O724 C725 110.04(12) . . ?
O724 C725 C726 111.31(14) . . ?
O724 C725 H72E 109.4 . . ?
C726 C725 H72E 109.4 . . ?
O724 C725 H72F 109.4 . . ?
C726 C725 H72F 109.4 . . ?
H72E C725 H72F 108 . . ?
N721 C726 C725 109.59(13) . . ?
N721 C726 H72G 109.8 . . ?
C725 C726 H72G 109.8 . . ?
N721 C726 H72H 109.8 . . ?
C725 C726 H72H 109.8 . . ?
H72G C726 H72H 108.2 . . ?
C74 C73 C72 120.86(14) . . ?
C74 C73 H73 119.6 . . ?
C72 C73 H73 119.6 . . ?
C73 C74 C74A 121.17(15) . . ?
C73 C74 H74 119.4 . . ?
C74A C74 H74 119.4 . . ?
C74 C74A C75 122.00(15) . . ?
C74 C74A C78A 118.89(14) . . ?
C75 C74A C78A 119.04(15) . . ?
C76 C75 C74A 120.78(16) . . ?
C76 C75 H75 119.6 . . ?
C74A C75 H75 119.6 . . ?
C75 C76 C77 120.37(15) . . ?
C75 C76 H76 119.8 . . ?
C77 C76 H76 119.8 . . ?
C78 C77 C76 120.40(16) . . ?
C78 C77 H77 119.8 . . ?
C76 C77 H77 119.8 . . ?
C77 C78 C78A 120.85(16) . . ?
C77 C78 H78 119.6 . . ?
C78A C78 H78 119.6 . . ?
C74A C78A C78 118.53(14) . . ?
C74A C78A C71 118.94(14) . . ?
C78 C78A C71 122.46(14) . . ?
N7 C8 C9 101.80(12) . . ?
N7 C8 H8A 111.4 . . ?
C9 C8 H8A 111.4 . . ?
N7 C8 H8B 111.4 . . ?
C9 C8 H8B 111.4 . . ?
H8A C8 H8B 109.3 . . ?
N10 C9 C8 101.48(12) . . ?
N10 C9 H9A 111.5 . . ?
C8 C9 H9A 111.5 . . ?
N10 C9 H9B 111.5 . . ?
C8 C9 H9B 111.5 . . ?
H9A C9 H9B 109.3 . . ?
C6 N10 C101 126.26(13) . . ?
C6 N10 C9 115.64(12) . . ?
C101 N10 C9 117.10(12) . . ?
C102 C101 C10B 121.26(14) . . ?
C102 C101 N10 119.43(13) . . ?
C10B C101 N10 118.87(13) . . ?
C101 C102 N111 118.88(14) . . ?
C101 C102 C103 118.55(15) . . ?
N111 C102 C103 122.55(14) . . ?
C102 N111 C112 117.68(13) . . ?
C102 N111 C116 114.69(12) . . ?
C112 N111 C116 109.16(13) . . ?
N111 C112 C113 108.22(15) . . ?
N111 C112 H11A 110.1 . . ?
C113 C112 H11A 110.1 . . ?
N111 C112 H11B 110.1 . . ?
C113 C112 H11B 110.1 . . ?
H11A C112 H11B 108.4 . . ?
O114 C113 C112 111.87(15) . . ?
O114 C113 H11C 109.2 . . ?
C112 C113 H11C 109.2 . . ?
O114 C113 H11D 109.2 . . ?
C112 C113 H11D 109.2 . . ?
H11C C113 H11D 107.9 . . ?
C115 O114 C113 110.49(13) . . ?
O114 C115 C116 111.33(14) . . ?
O114 C115 H11E 109.4 . . ?
C116 C115 H11E 109.4 . . ?
O114 C115 H11F 109.4 . . ?
C116 C115 H11F 109.4 . . ?
H11E C115 H11F 108 . . ?
N111 C116 C115 109.22(13) . . ?
N111 C116 H11G 109.8 . . ?
C115 C116 H11G 109.8 . . ?
N111 C116 H11H 109.8 . . ?
C115 C116 H11H 109.8 . . ?
H11G C116 H11H 108.3 . . ?
C104 C103 C102 121.28(15) . . ?
C104 C103 H103 119.4 . . ?
C102 C103 H103 119.4 . . ?
C103 C104 C10A 121.39(15) . . ?
C103 C104 H104 119.3 . . ?
C10A C104 H104 119.3 . . ?
C104 C10A C105 122.55(16) . . ?
C104 C10A C10B 118.59(15) . . ?
C105 C10A C10B 118.86(16) . . ?
C106 C105 C10A 120.90(17) . . ?
C106 C105 H105 119.6 . . ?
C10A C105 H105 119.6 . . ?
C105 C106 C107 120.50(17) . . ?
C105 C106 H106 119.8 . . ?
C107 C106 H106 119.8 . . ?
C108 C107 C106 120.31(17) . . ?
C108 C107 H107 119.8 . . ?
C106 C107 H107 119.8 . . ?
C107 C108 C10B 120.74(16) . . ?
C107 C108 H108 119.6 . . ?
C10B C108 H108 119.6 . . ?
C108 C10B C101 122.46(14) . . ?
C108 C10B C10A 118.69(15) . . ?
C101 C10B C10A 118.84(14) . . ?

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

data_rda601
_database_code_depnum_ccdc_archive 'CCDC 1518959'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2015-12-11T14:32:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C33 H36 N4'
_chemical_formula_moiety         'C33 H36 N4'
_chemical_formula_weight         488.66

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.68922(11)
_cell_length_b                   10.80236(10)
_cell_length_c                   23.3349(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.3129(10)
_cell_angle_gamma                90
_cell_volume                     2686.82(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16407
_cell_measurement_theta_min      3.793
_cell_measurement_theta_max      67.242

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

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             1048

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

_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
       CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_absorpt_correction_T_min  0.95005
_exptl_absorpt_correction_T_max  1

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

_diffrn_source                   'sealed X-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      -0.0094811
_diffrn_orient_matrix_ub_12      -0.0350354
_diffrn_orient_matrix_ub_13      0.0635438
_diffrn_orient_matrix_ub_21      0.1179071
_diffrn_orient_matrix_ub_22      0.0778557
_diffrn_orient_matrix_ub_23      0.0168747
_diffrn_orient_matrix_ub_31      -0.0830967
_diffrn_orient_matrix_ub_32      0.1141558
_diffrn_orient_matrix_ub_33      0.0079682
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_number            30335
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.799
_diffrn_reflns_theta_max         67.394
_diffrn_reflns_theta_full        67.394
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_number_total             4806
_reflns_number_gt                4268
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'

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

_atom_sites_solution_hydrogens   geom

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0719P)²+0.6674P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4806
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_restrained_S_all      0.99
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.042

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.40839(10) 0.40089(11) 0.34081(5) 0.0256(3) Uani 1 d . .
N2 N 0.42729(9) 0.40340(9) 0.39843(4) 0.0239(2) Uani 1 d . .
C21 C 0.52127(11) 0.33753(11) 0.43206(5) 0.0254(3) Uani 1 d . .
C22 C 0.48560(11) 0.24656(11) 0.46951(5) 0.0272(3) Uani 1 d . .
N221 N 0.35708(9) 0.21538(9) 0.46919(4) 0.0268(2) Uani 1 d . .
C222 C 0.31393(12) 0.16133(12) 0.52181(5) 0.0337(3) Uani 1 d . .
H22A H 0.3503 0.2076 0.5557 0.04 Uiso 1 calc . .
H22B H 0.3419 0.0741 0.5255 0.04 Uiso 1 calc . .
C223 C 0.17173(13) 0.16731(13) 0.51946(6) 0.0369(3) Uani 1 d . .
H22C H 0.1448 0.255 0.519 0.044 Uiso 1 calc . .
H22D H 0.1423 0.1281 0.5544 0.044 Uiso 1 calc . .
C224 C 0.11200(13) 0.10208(13) 0.46646(6) 0.0355(3) Uani 1 d . .
H22E H 0.1276 0.0119 0.4697 0.043 Uiso 1 calc . .
H22F H 0.0201 0.1156 0.4639 0.043 Uiso 1 calc . .
C225 C 0.16631(12) 0.15149(12) 0.41230(5) 0.0321(3) Uani 1 d . .
H22G H 0.1345 0.1014 0.3788 0.039 Uiso 1 calc . .
H22H H 0.1387 0.2381 0.4056 0.039 Uiso 1 calc . .
C226 C 0.30855(11) 0.14634(11) 0.41819(5) 0.0287(3) Uani 1 d . .
H22I H 0.3364 0.0591 0.4215 0.034 Uiso 1 calc . .
H22J H 0.3423 0.1823 0.3835 0.034 Uiso 1 calc . .
C23 C 0.57799(12) 0.18985(12) 0.50760(6) 0.0332(3) Uani 1 d . .
H23 H 0.5539 0.1281 0.5336 0.04 Uiso 1 calc . .
C24 C 0.70096(13) 0.22281(12) 0.50735(6) 0.0371(3) Uani 1 d . .
H24 H 0.7612 0.1835 0.5333 0.045 Uiso 1 calc . .
C24A C 0.74076(12) 0.31373(13) 0.46958(6) 0.0358(3) Uani 1 d . .
C25 C 0.86724(13) 0.35244(15) 0.47026(7) 0.0463(4) Uani 1 d . .
H25 H 0.9289 0.3132 0.4955 0.056 Uiso 1 calc . .
C26 C 0.90189(13) 0.44501(18) 0.43525(7) 0.0530(4) Uani 1 d . .
H26 H 0.9873 0.4698 0.4363 0.064 Uiso 1 calc . .
C27 C 0.81185(13) 0.50438(16) 0.39739(7) 0.0477(4) Uani 1 d . .
H27 H 0.837 0.569 0.3732 0.057 Uiso 1 calc . .
C28 C 0.68855(12) 0.46942(13) 0.39533(6) 0.0361(3) Uani 1 d . .
H28 H 0.6287 0.5102 0.3698 0.043 Uiso 1 calc . .
C28A C 0.64942(11) 0.37292(12) 0.43102(5) 0.0295(3) Uani 1 d . .
C3 C 0.34988(11) 0.49477(11) 0.42754(5) 0.0264(3) Uani 1 d . .
H3A H 0.4016 0.5638 0.4442 0.032 Uiso 1 calc . .
H3B H 0.3043 0.4554 0.4581 0.032 Uiso 1 calc . .
C4 C 0.26001(11) 0.53864(11) 0.37784(5) 0.0271(3) Uani 1 d . .
H4A H 0.1736 0.5085 0.3818 0.032 Uiso 1 calc . .
H4B H 0.259 0.6301 0.3749 0.032 Uiso 1 calc . .
N5 N 0.31494(9) 0.48147(9) 0.32773(4) 0.0246(2) Uani 1 d . .
C51 C 0.25839(10) 0.50377(11) 0.27118(5) 0.0263(3) Uani 1 d . .
C52 C 0.27126(11) 0.61933(11) 0.24627(5) 0.0276(3) Uani 1 d . .
N521 N 0.34113(10) 0.71203(9) 0.27648(4) 0.0292(2) Uani 1 d . .
C522 C 0.30986(13) 0.84091(11) 0.26192(6) 0.0339(3) Uani 1 d . .
H52A H 0.2178 0.8504 0.2552 0.041 Uiso 1 calc . .
H52B H 0.3488 0.8651 0.2264 0.041 Uiso 1 calc . .
C523 C 0.35897(13) 0.92283(12) 0.31166(6) 0.0381(3) Uani 1 d . .
H52C H 0.3408 1.0105 0.3019 0.046 Uiso 1 calc . .
H52D H 0.3151 0.9019 0.3463 0.046 Uiso 1 calc . .
C524 C 0.49935(14) 0.90643(13) 0.32473(6) 0.0398(3) Uani 1 d . .
H52E H 0.5265 0.9527 0.3601 0.048 Uiso 1 calc . .
H52F H 0.5442 0.9412 0.2928 0.048 Uiso 1 calc . .
C525 C 0.53391(12) 0.77000(12) 0.33273(6) 0.0348(3) Uani 1 d . .
H52G H 0.6263 0.761 0.3358 0.042 Uiso 1 calc . .
H52H H 0.502 0.739 0.3688 0.042 Uiso 1 calc . .
C526 C 0.47825(11) 0.69371(12) 0.28239(5) 0.0307(3) Uani 1 d . .
H52I H 0.5152 0.7197 0.2466 0.037 Uiso 1 calc . .
H52J H 0.4977 0.605 0.289 0.037 Uiso 1 calc . .
C53 C 0.21009(12) 0.64177(12) 0.19099(5) 0.0318(3) Uani 1 d . .
H53 H 0.2205 0.7195 0.1729 0.038 Uiso 1 calc . .
C54 C 0.13687(12) 0.55362(13) 0.16368(5) 0.0332(3) Uani 1 d . .
H54 H 0.0977 0.5708 0.1266 0.04 Uiso 1 calc . .
C54A C 0.11772(11) 0.43733(13) 0.18905(5) 0.0311(3) Uani 1 d . .
C55 C 0.03485(12) 0.34729(14) 0.16333(6) 0.0364(3) Uani 1 d . .
H55 H -0.0094 0.3649 0.1274 0.044 Uiso 1 calc . .
C56 C 0.01744(12) 0.23625(14) 0.18908(6) 0.0411(3) Uani 1 d . .
H56 H -0.0393 0.1776 0.1713 0.049 Uiso 1 calc . .
C57 C 0.08334(13) 0.20797(14) 0.24202(6) 0.0392(3) Uani 1 d . .
H57 H 0.0719 0.1298 0.2595 0.047 Uiso 1 calc . .
C58 C 0.16368(12) 0.29256(12) 0.26837(5) 0.0330(3) Uani 1 d . .
H58 H 0.2078 0.2722 0.304 0.04 Uiso 1 calc . .
C58A C 0.18214(11) 0.41025(12) 0.24336(5) 0.0281(3) Uani 1 d . .



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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N5 1.3426(15) . ?
C1 N2 1.3447(15) . ?
N2 C21 1.4187(15) . ?
N2 C3 1.4850(14) . ?
C21 C22 1.3875(18) . ?
C21 C28A 1.4242(17) . ?
C22 N221 1.4139(16) . ?
C22 C23 1.4172(17) . ?
N221 C226 1.4659(15) . ?
N221 C222 1.4651(16) . ?
C222 C223 1.5183(19) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 C224 1.5214(18) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
C224 C225 1.5263(18) . ?
C224 H22E 0.99 . ?
C224 H22F 0.99 . ?
C225 C226 1.5174(17) . ?
C225 H22G 0.99 . ?
C225 H22H 0.99 . ?
C226 H22I 0.99 . ?
C226 H22J 0.99 . ?
C23 C24 1.3623(19) . ?
C23 H23 0.95 . ?
C24 C24A 1.407(2) . ?
C24 H24 0.95 . ?
C24A C25 1.4142(19) . ?
C24A C28A 1.4282(18) . ?
C25 C26 1.360(2) . ?
C25 H25 0.95 . ?
C26 C27 1.411(2) . ?
C26 H26 0.95 . ?
C27 C28 1.3684(19) . ?
C27 H27 0.95 . ?
C28 C28A 1.4168(19) . ?
C28 H28 0.95 . ?
C3 C4 1.5248(16) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.4822(15) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.4299(14) . ?
C51 C52 1.3882(18) . ?
C51 C58A 1.4236(17) . ?
C52 N521 1.4065(16) . ?
C52 C53 1.4225(17) . ?
N521 C522 1.4657(16) . ?
N521 C526 1.4752(16) . ?
C522 C523 1.5213(18) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 C524 1.519(2) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
C524 C525 1.527(2) . ?
C524 H52E 0.99 . ?
C524 H52F 0.99 . ?
C525 C526 1.5193(17) . ?
C525 H52G 0.99 . ?
C525 H52H 0.99 . ?
C526 H52I 0.99 . ?
C526 H52J 0.99 . ?
C53 C54 1.3604(19) . ?
C53 H53 0.95 . ?
C54 C54A 1.4103(19) . ?
C54 H54 0.95 . ?
C54A C55 1.4181(18) . ?
C54A C58A 1.4264(17) . ?
C55 C56 1.361(2) . ?
C55 H55 0.95 . ?
C56 C57 1.409(2) . ?
C56 H56 0.95 . ?
C57 C58 1.3678(18) . ?
C57 H57 0.95 . ?
C58 C58A 1.4188(18) . ?
C58 H58 0.95 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 C1 N2 105.52(10) . . ?
C1 N2 C21 126.15(10) . . ?
C1 N2 C3 115.07(9) . . ?
C21 N2 C3 118.43(9) . . ?
C22 C21 N2 119.14(10) . . ?
C22 C21 C28A 120.74(11) . . ?
N2 C21 C28A 119.86(11) . . ?
C21 C22 N221 118.57(10) . . ?
C21 C22 C23 119.31(11) . . ?
N221 C22 C23 122.10(11) . . ?
C22 N221 C226 114.20(9) . . ?
C22 N221 C222 117.22(10) . . ?
C226 N221 C222 111.29(9) . . ?
N221 C222 C223 109.28(10) . . ?
N221 C222 H22A 109.8 . . ?
C223 C222 H22A 109.8 . . ?
N221 C222 H22B 109.8 . . ?
C223 C222 H22B 109.8 . . ?
H22A C222 H22B 108.3 . . ?
C222 C223 C224 111.56(11) . . ?
C222 C223 H22C 109.3 . . ?
C224 C223 H22C 109.3 . . ?
C222 C223 H22D 109.3 . . ?
C224 C223 H22D 109.3 . . ?
H22C C223 H22D 108 . . ?
C225 C224 C223 110.41(10) . . ?
C225 C224 H22E 109.6 . . ?
C223 C224 H22E 109.6 . . ?
C225 C224 H22F 109.6 . . ?
C223 C224 H22F 109.6 . . ?
H22E C224 H22F 108.1 . . ?
C226 C225 C224 110.67(10) . . ?
C226 C225 H22G 109.5 . . ?
C224 C225 H22G 109.5 . . ?
C226 C225 H22H 109.5 . . ?
C224 C225 H22H 109.5 . . ?
H22G C225 H22H 108.1 . . ?
N221 C226 C225 110.24(10) . . ?
N221 C226 H22I 109.6 . . ?
C225 C226 H22I 109.6 . . ?
N221 C226 H22J 109.6 . . ?
C225 C226 H22J 109.6 . . ?
H22I C226 H22J 108.1 . . ?
C24 C23 C22 120.77(13) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C24A 121.49(12) . . ?
C23 C24 H24 119.3 . . ?
C24A C24 H24 119.3 . . ?
C24 C24A C25 122.23(13) . . ?
C24 C24A C28A 118.87(12) . . ?
C25 C24A C28A 118.84(14) . . ?
C26 C25 C24A 120.92(14) . . ?
C26 C25 H25 119.5 . . ?
C24A C25 H25 119.5 . . ?
C25 C26 C27 120.44(13) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 120.43(15) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C28A 120.57(13) . . ?
C27 C28 H28 119.7 . . ?
C28A C28 H28 119.7 . . ?
C28 C28A C21 122.30(11) . . ?
C28 C28A C24A 118.80(12) . . ?
C21 C28A C24A 118.81(12) . . ?
N2 C3 C4 101.50(9) . . ?
N2 C3 H3A 111.5 . . ?
C4 C3 H3A 111.5 . . ?
N2 C3 H3B 111.5 . . ?
C4 C3 H3B 111.5 . . ?
H3A C3 H3B 109.3 . . ?
N5 C4 C3 101.90(9) . . ?
N5 C4 H4A 111.4 . . ?
C3 C4 H4A 111.4 . . ?
N5 C4 H4B 111.4 . . ?
C3 C4 H4B 111.4 . . ?
H4A C4 H4B 109.3 . . ?
C1 N5 C51 125.08(10) . . ?
C1 N5 C4 115.01(9) . . ?
C51 N5 C4 119.52(9) . . ?
C52 C51 C58A 121.23(11) . . ?
C52 C51 N5 119.31(10) . . ?
C58A C51 N5 119.28(11) . . ?
C51 C52 N521 119.73(10) . . ?
C51 C52 C53 118.67(11) . . ?
N521 C52 C53 121.58(11) . . ?
C52 N521 C522 117.18(10) . . ?
C52 N521 C526 115.96(10) . . ?
C522 N521 C526 110.90(10) . . ?
N521 C522 C523 108.43(10) . . ?
N521 C522 H52A 110 . . ?
C523 C522 H52A 110 . . ?
N521 C522 H52B 110 . . ?
C523 C522 H52B 110 . . ?
H52A C522 H52B 108.4 . . ?
C524 C523 C522 111.36(11) . . ?
C524 C523 H52C 109.4 . . ?
C522 C523 H52C 109.4 . . ?
C524 C523 H52D 109.4 . . ?
C522 C523 H52D 109.4 . . ?
H52C C523 H52D 108 . . ?
C523 C524 C525 111.30(11) . . ?
C523 C524 H52E 109.4 . . ?
C525 C524 H52E 109.4 . . ?
C523 C524 H52F 109.4 . . ?
C525 C524 H52F 109.4 . . ?
H52E C524 H52F 108 . . ?
C526 C525 C524 110.60(11) . . ?
C526 C525 H52G 109.5 . . ?
C524 C525 H52G 109.5 . . ?
C526 C525 H52H 109.5 . . ?
C524 C525 H52H 109.5 . . ?
H52G C525 H52H 108.1 . . ?
N521 C526 C525 109.15(10) . . ?
N521 C526 H52I 109.9 . . ?
C525 C526 H52I 109.9 . . ?
N521 C526 H52J 109.8 . . ?
C525 C526 H52J 109.9 . . ?
H52I C526 H52J 108.3 . . ?
C54 C53 C52 120.97(12) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C53 C54 C54A 121.56(11) . . ?
C53 C54 H54 119.2 . . ?
C54A C54 H54 119.2 . . ?
C54 C54A C55 122.61(12) . . ?
C54 C54A C58A 118.69(11) . . ?
C55 C54A C58A 118.68(12) . . ?
C56 C55 C54A 121.30(13) . . ?
C56 C55 H55 119.4 . . ?
C54A C55 H55 119.4 . . ?
C55 C56 C57 120.16(12) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C58 C57 C56 120.33(13) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C57 C58 C58A 121.05(12) . . ?
C57 C58 H58 119.5 . . ?
C58A C58 H58 119.5 . . ?
C58 C58A C51 122.75(11) . . ?
C58 C58A C54A 118.44(11) . . ?
C51 C58A C54A 118.76(12) . . ?

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

data_rda015
_database_code_depnum_ccdc_archive 'CCDC 1518960'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2012-06-04T09:49:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C40 H41 Cl N4 O2 Pd'
_chemical_formula_moiety         'C40 H41 Cl N4 O2 Pd'
_chemical_formula_weight         751.62

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-c 2yc'
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'
'-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                   33.1649(7)
_cell_length_b                   11.2485(2)
_cell_length_c                   18.6466(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.804(2)
_cell_angle_gamma                90
_cell_volume                     6783.2(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20310
_cell_measurement_theta_min      2.8352
_cell_measurement_theta_max      34.1391

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

_exptl_crystal_description       prism
_exptl_crystal_colour            pale_yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3104
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 1 0.0544
-1 -1 -1 0.0592
-1 1 -1 0.0676
1 -1 1 0.0704
1 0 0 0.0483
-1 0 0 0.0513

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
    CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
              model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

;
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_T_max  0.947

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      0.0042071
_diffrn_orient_matrix_ub_12      -0.0379092
_diffrn_orient_matrix_ub_13      0.0311636
_diffrn_orient_matrix_ub_21      0.0003918
_diffrn_orient_matrix_ub_22      -0.0497195
_diffrn_orient_matrix_ub_23      -0.0232302
_diffrn_orient_matrix_ub_31      0.0215304
_diffrn_orient_matrix_ub_32      0.0082322
_diffrn_orient_matrix_ub_33      0.003162
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.046
_diffrn_reflns_number            72176
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         33.5
_diffrn_reflns_theta_full        33.5
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             13266
_reflns_number_gt                10546
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

One morpholine group of one of the ligands and the phenylallyl group were both 
modelled as being disordered over two sets of sites. The occupancies of the
two components of the morpholine group were refined to 0.729(15) and its 
complement with those of the phenylallyl restrained to 0.5 after trial 
refinement.
Geometries of the disordered groups were restrained to ideal values.
;
_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)+(0.0379P)²+9.6743P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         13266
_refine_ls_number_parameters     530
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.074
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.088

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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 0.135913(5) 0.165113(15) 0.736498(8) 0.02439(5) Uani 1 1 d . . .
Cl1 Cl 0.13476(2) -0.02362(5) 0.79466(3) 0.03411(13) Uani 1 1 d . B .
C1 C 0.11881(7) 0.10680(19) 0.63067(11) 0.0239(4) Uani 1 1 d . B .
N2 N 0.14306(6) 0.11487(18) 0.58137(10) 0.0270(4) Uani 1 1 d . . .
C21 C 0.18108(7) 0.1791(2) 0.59144(12) 0.0270(4) Uani 1 1 d . A .
C22 C 0.18478(8) 0.2725(2) 0.54446(13) 0.0323(5) Uani 1 1 d . . .
N221 N 0.15367(19) 0.3122(5) 0.4877(3) 0.0267(10) Uani 0.729(15) 1 d PD A 1
C222 C 0.1177(2) 0.3659(9) 0.5079(4) 0.0295(12) Uani 0.729(15) 1 d PD A 1
H22A H 0.1245 0.4476 0.5265 0.035 Uiso 0.729(15) 1 calc PR A 1
H22B H 0.1097 0.3188 0.5473 0.035 Uiso 0.729(15) 1 calc PR A 1
C223 C 0.0824(2) 0.3694(6) 0.4411(4) 0.0425(13) Uani 0.729(15) 1 d PD A 1
H22C H 0.0751 0.2873 0.424 0.051 Uiso 0.729(15) 1 calc PR A 1
H22D H 0.0578 0.4055 0.4547 0.051 Uiso 0.729(15) 1 calc PR A 1
O224 O 0.09283(19) 0.4363(4) 0.3831(3) 0.0459(11) Uani 0.729(15) 1 d PD A 1
C225 C 0.1283(2) 0.3861(5) 0.3642(2) 0.0474(15) Uani 0.729(15) 1 d PD A 1
H22E H 0.1357 0.4334 0.3242 0.057 Uiso 0.729(15) 1 calc PR A 1
H22F H 0.1219 0.3041 0.3458 0.057 Uiso 0.729(15) 1 calc PR A 1
C226 C 0.16434(19) 0.3835(5) 0.4291(3) 0.0383(12) Uani 0.729(15) 1 d PD A 1
H22G H 0.1887 0.3488 0.4144 0.046 Uiso 0.729(15) 1 calc PR A 1
H22H H 0.1714 0.4654 0.4469 0.046 Uiso 0.729(15) 1 calc PR A 1
N231 N 0.1436(5) 0.2876(14) 0.4848(7) 0.025(3) Uani 0.271(15) 1 d PD A 2
C232 C 0.1137(6) 0.354(3) 0.5153(11) 0.0295(12) Uani 0.271(15) 1 d PDU A 2
H23A H 0.1243 0.4344 0.5298 0.035 Uiso 0.271(15) 1 calc PR A 2
H23B H 0.1086 0.3127 0.5594 0.035 Uiso 0.271(15) 1 calc PR A 2
C233 C 0.0740(5) 0.362(2) 0.4575(11) 0.0425(13) Uani 0.271(15) 1 d PDU A 2
H23C H 0.0618 0.2815 0.4483 0.051 Uiso 0.271(15) 1 calc PR A 2
H23D H 0.0541 0.4121 0.4764 0.051 Uiso 0.271(15) 1 calc PR A 2
O234 O 0.0795(5) 0.4104(13) 0.3899(8) 0.047(3) Uani 0.271(15) 1 d PDU A 2
C235 C 0.1096(6) 0.3447(17) 0.3625(6) 0.052(4) Uani 0.271(15) 1 d PDU A 2
H23E H 0.1136 0.3817 0.3164 0.063 Uiso 0.271(15) 1 calc PR A 2
H23F H 0.0995 0.2625 0.351 0.063 Uiso 0.271(15) 1 calc PR A 2
C236 C 0.1504(5) 0.3408(17) 0.4175(7) 0.046(3) Uani 0.271(15) 1 d PDU A 2
H23G H 0.1706 0.293 0.3978 0.055 Uiso 0.271(15) 1 calc PR A 2
H23H H 0.1615 0.4222 0.4274 0.055 Uiso 0.271(15) 1 calc PR A 2
C23 C 0.22297(9) 0.3344(2) 0.55497(16) 0.0406(6) Uani 1 1 d . A .
H23 H 0.226 0.3957 0.5216 0.049 Uiso 1 1 calc R . .
C24 C 0.25517(8) 0.3082(2) 0.61146(15) 0.0375(6) Uani 1 1 d . . .
H24 H 0.28 0.3528 0.6177 0.045 Uiso 1 1 calc R A .
C24A C 0.25223(7) 0.2157(2) 0.66094(13) 0.0294(5) Uani 1 1 d . A .
C25 C 0.28541(8) 0.1884(2) 0.72095(14) 0.0339(5) Uani 1 1 d . . .
H25 H 0.3096 0.2365 0.7301 0.041 Uiso 1 1 calc R A .
C26 C 0.28302(7) 0.0946(2) 0.76528(13) 0.0335(5) Uani 1 1 d . A .
H26 H 0.3053 0.0778 0.8057 0.04 Uiso 1 1 calc R . .
C27 C 0.24758(7) 0.0216(2) 0.75176(13) 0.0305(5) Uani 1 1 d . . .
H27 H 0.2467 -0.046 0.7819 0.037 Uiso 1 1 calc R A .
C28 C 0.21438(7) 0.0471(2) 0.69561(12) 0.0268(4) Uani 1 1 d . A .
H28 H 0.1906 -0.0022 0.6878 0.032 Uiso 1 1 calc R . .
C28A C 0.21527(7) 0.14613(19) 0.64920(12) 0.0243(4) Uani 1 1 d . . .
C3 C 0.12579(8) 0.0508(2) 0.51165(12) 0.0336(5) Uani 1 1 d . B .
H3A H 0.1417 -0.0224 0.5074 0.04 Uiso 1 1 calc R . .
H3B H 0.1254 0.102 0.4683 0.04 Uiso 1 1 calc R . .
C4 C 0.08239(8) 0.0221(2) 0.51980(12) 0.0342(5) Uani 1 1 d . . .
H4A H 0.0617 0.0725 0.4871 0.041 Uiso 1 1 calc R B .
H4B H 0.0756 -0.0626 0.5087 0.041 Uiso 1 1 calc R . .
N5 N 0.08413(6) 0.04901(17) 0.59815(9) 0.0251(4) Uani 1 1 d . B .
C51 C 0.04727(7) 0.0344(2) 0.62519(11) 0.0257(4) Uani 1 1 d . . .
C52 C 0.03236(7) -0.0784(2) 0.63162(11) 0.0279(4) Uani 1 1 d . B .
N521 N 0.05515(6) -0.17938(17) 0.61565(11) 0.0312(4) Uani 1 1 d . . .
C522 C 0.07382(10) -0.2486(2) 0.68094(15) 0.0439(7) Uani 1 1 d . B .
H52A H 0.052 -0.2863 0.7017 0.053 Uiso 1 1 calc R . .
H52B H 0.0904 -0.196 0.7189 0.053 Uiso 1 1 calc R . .
C523 C 0.10117(11) -0.3427(3) 0.65877(19) 0.0581(9) Uani 1 1 d . . .
H52C H 0.1233 -0.304 0.6393 0.07 Uiso 1 1 calc R B .
H52D H 0.1144 -0.3898 0.7026 0.07 Uiso 1 1 calc R . .
O524 O 0.07802(8) -0.42038(18) 0.60403(11) 0.0548(6) Uani 1 1 d . B .
C525 C 0.05863(11) -0.3537(3) 0.54139(16) 0.0511(8) Uani 1 1 d . . .
H52G H 0.0421 -0.4078 0.5044 0.061 Uiso 1 1 calc R B .
H52H H 0.0801 -0.3167 0.5193 0.061 Uiso 1 1 calc R . .
C526 C 0.03102(9) -0.2582(3) 0.56026(15) 0.0445(7) Uani 1 1 d . B .
H52I H 0.0186 -0.2122 0.5156 0.053 Uiso 1 1 calc R . .
H52J H 0.0084 -0.2948 0.5794 0.053 Uiso 1 1 calc R . .
C53 C -0.00570(8) -0.0933(2) 0.65290(12) 0.0322(5) Uani 1 1 d . . .
H53 H -0.0154 -0.1714 0.659 0.039 Uiso 1 1 calc R B .
C54 C -0.02873(8) 0.0011(2) 0.66482(12) 0.0327(5) Uani 1 1 d . B .
H54 H -0.0542 -0.0114 0.6788 0.039 Uiso 1 1 calc R . .
C54A C -0.01493(7) 0.1179(2) 0.65651(12) 0.0304(5) Uani 1 1 d . . .
C55 C -0.03917(9) 0.2181(3) 0.66652(14) 0.0394(6) Uani 1 1 d . B .
H55 H -0.065 0.2063 0.6795 0.047 Uiso 1 1 calc R . .
C56 C -0.02615(9) 0.3303(3) 0.65793(15) 0.0421(6) Uani 1 1 d . . .
H56 H -0.0428 0.3961 0.6652 0.05 Uiso 1 1 calc R B .
C57 C 0.01212(9) 0.3497(2) 0.63819(13) 0.0374(6) Uani 1 1 d . B .
H57 H 0.0211 0.4285 0.6319 0.045 Uiso 1 1 calc R . .
C58 C 0.03630(8) 0.2550(2) 0.62806(12) 0.0295(5) Uani 1 1 d . . .
H58 H 0.0619 0.2692 0.6149 0.035 Uiso 1 1 calc R B .
C58A C 0.02388(7) 0.1364(2) 0.63687(11) 0.0266(4) Uani 1 1 d . B .
C11 C 0.15001(14) 0.2801(4) 0.8418(2) 0.0267(6) Uani 0.5 1 d P B 1
H11 H 0.1207 0.2824 0.8327 0.032 Uiso 0.5 1 calc PR B 1
C12 C 0.16990(18) 0.3205(4) 0.7851(3) 0.0304(8) Uani 0.5 1 d P B 1
H12 H 0.1991 0.3294 0.794 0.036 Uiso 0.5 1 calc PR B 1
C13 C 0.14424(8) 0.3466(2) 0.71507(14) 0.0333(5) Uani 1 1 d . B .
H13A H 0.1151 0.3371 0.7072 0.04 Uiso 0.5 1 calc PR C 1
H13B H 0.1562 0.3734 0.6762 0.04 Uiso 0.5 1 calc PR C 1
H13C H 0.1641 0.3088 0.693 0.04 Uiso 0.5 1 d PR C 2
H13D H 0.1235 0.3956 0.6863 0.04 Uiso 0.5 1 d PR C 2
C11' C 0.17624(14) 0.2580(4) 0.8319(2) 0.0267(6) Uani 0.5 1 d P B 2
H11' H 0.1962 0.2232 0.8088 0.032 Uiso 0.5 1 calc PR B 2
C12' C 0.14907(17) 0.3280(5) 0.7910(3) 0.0304(8) Uani 0.5 1 d P B 2
H12' H 0.1309 0.3701 0.8148 0.036 Uiso 0.5 1 calc PR B 2
C101 C 0.1732(15) 0.235(5) 0.9135(7) 0.030(2) Uani 0.5 1 d PD B 1
C102 C 0.1630(3) 0.2644(9) 0.9794(4) 0.0360(17) Uani 0.5 1 d PD B 1
H102 H 0.1397 0.3137 0.9792 0.043 Uiso 0.5 1 calc PR B 1
C103 C 0.1862(3) 0.2224(10) 1.0456(4) 0.049(3) Uani 0.5 1 d PD B 1
H103 H 0.179 0.2451 1.0902 0.059 Uiso 0.5 1 calc PR B 1
C104 C 0.2187(3) 0.1504(8) 1.0480(4) 0.048(2) Uani 0.5 1 d PD B 1
H104 H 0.2347 0.124 1.094 0.058 Uiso 0.5 1 calc PR B 1
C105 C 0.2292(2) 0.1140(6) 0.9825(4) 0.0405(14) Uani 0.5 1 d PD B 1
H105 H 0.2516 0.061 0.9835 0.049 Uiso 0.5 1 calc PR B 1
C106 C 0.2057(3) 0.1575(8) 0.9149(3) 0.0320(15) Uani 0.5 1 d PD B 1
H106 H 0.2123 0.1331 0.87 0.038 Uiso 0.5 1 calc PR B 1
C201 C 0.1795(15) 0.227(5) 0.9103(7) 0.030(2) Uani 0.5 1 d PD B 2
C202 C 0.1612(3) 0.2934(10) 0.9574(5) 0.045(2) Uani 0.5 1 d PD B 2
H202 H 0.1407 0.351 0.938 0.054 Uiso 0.5 1 calc PR B 2
C203 C 0.1729(3) 0.2756(8) 1.0322(4) 0.0444(17) Uani 0.5 1 d PD B 2
H203 H 0.1608 0.3234 1.0638 0.053 Uiso 0.5 1 calc PR B 2
C204 C 0.2010(4) 0.1920(10) 1.0623(5) 0.044(2) Uani 0.5 1 d PD B 2
H204 H 0.2082 0.1807 1.114 0.053 Uiso 0.5 1 calc PR B 2
C205 C 0.2193(2) 0.1228(6) 1.0161(6) 0.0436(17) Uani 0.5 1 d PD B 2
H205 H 0.2387 0.0629 1.0363 0.052 Uiso 0.5 1 calc PR B 2
C206 C 0.2090(2) 0.1417(7) 0.9397(4) 0.0304(15) Uani 0.5 1 d PD B 2
H206 H 0.2222 0.0966 0.9084 0.037 Uiso 0.5 1 calc PR B 2



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 2.037(2) . ?
Pd1 C12' 2.093(5) . ?
Pd1 C13 2.110(2) . ?
Pd1 C12 2.166(5) . ?
Pd1 C11' 2.234(4) . ?
Pd1 C11 2.311(4) . ?
Pd1 Cl1 2.3880(6) . ?
C1 N5 1.343(3) . ?
C1 N2 1.352(3) . ?
N2 C21 1.429(3) . ?
N2 C3 1.486(3) . ?
C21 C22 1.390(3) . ?
C21 C28A 1.429(3) . ?
C22 N221 1.378(6) . ?
C22 C23 1.420(4) . ?
C22 N231 1.567(14) . ?
N221 C222 1.459(6) . ?
N221 C226 1.461(6) . ?
C222 C223 1.510(6) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 O224 1.423(6) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
O224 C225 1.418(6) . ?
C225 C226 1.501(6) . ?
C225 H22E 0.99 . ?
C225 H22F 0.99 . ?
C226 H22G 0.99 . ?
C226 H22H 0.99 . ?
N231 C236 1.452(13) . ?
N231 C232 1.454(15) . ?
C232 C233 1.508(15) . ?
C232 H23A 0.99 . ?
C232 H23B 0.99 . ?
C233 O234 1.421(14) . ?
C233 H23C 0.99 . ?
C233 H23D 0.99 . ?
O234 C235 1.425(14) . ?
C235 C236 1.505(14) . ?
C235 H23E 0.99 . ?
C235 H23F 0.99 . ?
C236 H23G 0.99 . ?
C236 H23H 0.99 . ?
C23 C24 1.356(4) . ?
C23 H23 0.95 . ?
C24 C24A 1.408(3) . ?
C24 H24 0.95 . ?
C24A C25 1.418(3) . ?
C24A C28A 1.430(3) . ?
C25 C26 1.354(4) . ?
C25 H25 0.95 . ?
C26 C27 1.410(3) . ?
C26 H26 0.95 . ?
C27 C28 1.371(3) . ?
C27 H27 0.95 . ?
C28 C28A 1.415(3) . ?
C28 H28 0.95 . ?
C3 C4 1.515(4) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.481(3) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.431(3) . ?
C51 C52 1.377(3) . ?
C51 C58A 1.428(3) . ?
C52 C53 1.415(3) . ?
C52 N521 1.431(3) . ?
N521 C526 1.459(3) . ?
N521 C522 1.462(3) . ?
C522 C523 1.511(4) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 O524 1.431(4) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
O524 C525 1.417(4) . ?
C525 C526 1.503(4) . ?
C525 H52G 0.99 . ?
C525 H52H 0.99 . ?
C526 H52I 0.99 . ?
C526 H52J 0.99 . ?
C53 C54 1.355(4) . ?
C53 H53 0.95 . ?
C54 C54A 1.411(4) . ?
C54 H54 0.95 . ?
C54A C55 1.421(4) . ?
C54A C58A 1.430(3) . ?
C55 C56 1.354(4) . ?
C55 H55 0.95 . ?
C56 C57 1.415(4) . ?
C56 H56 0.95 . ?
C57 C58 1.372(3) . ?
C57 H57 0.95 . ?
C58 C58A 1.416(3) . ?
C58 H58 0.95 . ?
C11 C12 1.438(7) . ?
C11 C101 1.475(13) . ?
C11 H11 0.95 . ?
C12 C13 1.422(6) . ?
C12 H12 0.95 . ?
C13 C12' 1.404(6) . ?
C13 H13A 0.95 . ?
C13 H13B 0.95 . ?
C13 H13C 0.95 . ?
C13 H13D 0.95 . ?
C11' C12' 1.308(7) . ?
C11' C201 1.48(2) . ?
C11' H11' 0.95 . ?
C12' H12' 0.95 . ?
C101 C106 1.384(11) . ?
C101 C102 1.385(11) . ?
C102 C103 1.387(11) . ?
C102 H102 0.95 . ?
C103 C104 1.341(13) . ?
C103 H103 0.95 . ?
C104 C105 1.403(10) . ?
C104 H104 0.95 . ?
C105 C106 1.414(8) . ?
C105 H105 0.95 . ?
C106 H106 0.95 . ?
C201 C206 1.390(12) . ?
C201 C202 1.394(11) . ?
C202 C203 1.378(9) . ?
C202 H202 0.95 . ?
C203 C204 1.356(11) . ?
C203 H203 0.95 . ?
C204 C205 1.395(12) . ?
C204 H204 0.95 . ?
C205 C206 1.405(10) . ?
C205 H205 0.95 . ?
C206 H206 0.95 . ?

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 C12' 137.33(16) . . ?
C1 Pd1 C13 98.52(9) . . ?
C12' Pd1 C13 39.04(16) . . ?
C1 Pd1 C12 132.23(16) . . ?
C13 Pd1 C12 38.81(16) . . ?
C1 Pd1 C11' 155.66(14) . . ?
C12' Pd1 C11' 34.99(19) . . ?
C13 Pd1 C11' 67.55(14) . . ?
C1 Pd1 C11 164.52(13) . . ?
C13 Pd1 C11 66.98(14) . . ?
C12 Pd1 C11 37.31(18) . . ?
C1 Pd1 Cl1 97.16(6) . . ?
C12' Pd1 Cl1 125.46(15) . . ?
C13 Pd1 Cl1 164.16(7) . . ?
C12 Pd1 Cl1 125.91(14) . . ?
C11' Pd1 Cl1 96.95(12) . . ?
C11 Pd1 Cl1 97.61(12) . . ?
N5 C1 N2 107.73(18) . . ?
N5 C1 Pd1 128.32(16) . . ?
N2 C1 Pd1 123.85(16) . . ?
C1 N2 C21 125.81(18) . . ?
C1 N2 C3 112.97(19) . . ?
C21 N2 C3 121.21(19) . . ?
C22 C21 C28A 120.3(2) . . ?
C22 C21 N2 119.9(2) . . ?
C28A C21 N2 119.8(2) . . ?
N221 C22 C21 124.9(3) . . ?
N221 C22 C23 116.1(3) . . ?
C21 C22 C23 118.9(2) . . ?
C21 C22 N231 110.2(6) . . ?
C23 C22 N231 130.9(6) . . ?
C22 N221 C222 116.9(5) . . ?
C22 N221 C226 119.2(4) . . ?
C222 N221 C226 108.2(5) . . ?
N221 C222 C223 109.2(5) . . ?
N221 C222 H22A 109.8 . . ?
C223 C222 H22A 109.8 . . ?
N221 C222 H22B 109.8 . . ?
C223 C222 H22B 109.8 . . ?
H22A C222 H22B 108.3 . . ?
O224 C223 C222 111.4(4) . . ?
O224 C223 H22C 109.3 . . ?
C222 C223 H22C 109.3 . . ?
O224 C223 H22D 109.3 . . ?
C222 C223 H22D 109.3 . . ?
H22C C223 H22D 108 . . ?
C225 O224 C223 109.5(4) . . ?
O224 C225 C226 111.3(4) . . ?
O224 C225 H22E 109.4 . . ?
C226 C225 H22E 109.4 . . ?
O224 C225 H22F 109.4 . . ?
C226 C225 H22F 109.4 . . ?
H22E C225 H22F 108 . . ?
N221 C226 C225 109.5(4) . . ?
N221 C226 H22G 109.8 . . ?
C225 C226 H22G 109.8 . . ?
N221 C226 H22H 109.8 . . ?
C225 C226 H22H 109.8 . . ?
H22G C226 H22H 108.2 . . ?
C236 N231 C232 112.1(13) . . ?
C236 N231 C22 112.5(9) . . ?
C232 N231 C22 110.0(12) . . ?
N231 C232 C233 108.5(15) . . ?
N231 C232 H23A 110 . . ?
C233 C232 H23A 110 . . ?
N231 C232 H23B 110 . . ?
C233 C232 H23B 110 . . ?
H23A C232 H23B 108.4 . . ?
O234 C233 C232 113.1(13) . . ?
O234 C233 H23C 109 . . ?
C232 C233 H23C 109 . . ?
O234 C233 H23D 109 . . ?
C232 C233 H23D 109 . . ?
H23C C233 H23D 107.8 . . ?
C233 O234 C235 110.9(11) . . ?
O234 C235 C236 111.4(10) . . ?
O234 C235 H23E 109.3 . . ?
C236 C235 H23E 109.3 . . ?
O234 C235 H23F 109.3 . . ?
C236 C235 H23F 109.3 . . ?
H23E C235 H23F 108 . . ?
N231 C236 C235 108.3(11) . . ?
N231 C236 H23G 110 . . ?
C235 C236 H23G 110 . . ?
N231 C236 H23H 110 . . ?
C235 C236 H23H 110 . . ?
H23G C236 H23H 108.4 . . ?
C24 C23 C22 121.7(2) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C24A 120.8(2) . . ?
C23 C24 H24 119.6 . . ?
C24A C24 H24 119.6 . . ?
C24 C24A C25 121.5(2) . . ?
C24 C24A C28A 119.1(2) . . ?
C25 C24A C28A 119.4(2) . . ?
C26 C25 C24A 120.7(2) . . ?
C26 C25 H25 119.7 . . ?
C24A C25 H25 119.7 . . ?
C25 C26 C27 120.3(2) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 120.8(2) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C28A 120.6(2) . . ?
C27 C28 H28 119.7 . . ?
C28A C28 H28 119.7 . . ?
C28 C28A C21 123.0(2) . . ?
C28 C28A C24A 118.1(2) . . ?
C21 C28A C24A 118.9(2) . . ?
N2 C3 C4 101.91(18) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.3 . . ?
N5 C4 C3 103.01(18) . . ?
N5 C4 H4A 111.2 . . ?
C3 C4 H4A 111.2 . . ?
N5 C4 H4B 111.2 . . ?
C3 C4 H4B 111.2 . . ?
H4A C4 H4B 109.1 . . ?
C1 N5 C51 127.53(18) . . ?
C1 N5 C4 112.76(19) . . ?
C51 N5 C4 118.33(17) . . ?
C52 C51 C58A 120.6(2) . . ?
C52 C51 N5 119.2(2) . . ?
C58A C51 N5 119.8(2) . . ?
C51 C52 C53 119.5(2) . . ?
C51 C52 N521 119.8(2) . . ?
C53 C52 N521 120.6(2) . . ?
C52 N521 C526 113.42(19) . . ?
C52 N521 C522 113.3(2) . . ?
C526 N521 C522 109.3(2) . . ?
N521 C522 C523 108.3(2) . . ?
N521 C522 H52A 110 . . ?
C523 C522 H52A 110 . . ?
N521 C522 H52B 110 . . ?
C523 C522 H52B 110 . . ?
H52A C522 H52B 108.4 . . ?
O524 C523 C522 111.3(3) . . ?
O524 C523 H52C 109.4 . . ?
C522 C523 H52C 109.4 . . ?
O524 C523 H52D 109.4 . . ?
C522 C523 H52D 109.4 . . ?
H52C C523 H52D 108 . . ?
C525 O524 C523 109.8(2) . . ?
O524 C525 C526 112.0(2) . . ?
O524 C525 H52G 109.2 . . ?
C526 C525 H52G 109.2 . . ?
O524 C525 H52H 109.2 . . ?
C526 C525 H52H 109.2 . . ?
H52G C525 H52H 107.9 . . ?
N521 C526 C525 109.5(2) . . ?
N521 C526 H52I 109.8 . . ?
C525 C526 H52I 109.8 . . ?
N521 C526 H52J 109.8 . . ?
C525 C526 H52J 109.8 . . ?
H52I C526 H52J 108.2 . . ?
C54 C53 C52 121.6(2) . . ?
C54 C53 H53 119.2 . . ?
C52 C53 H53 119.2 . . ?
C53 C54 C54A 120.2(2) . . ?
C53 C54 H54 119.9 . . ?
C54A C54 H54 119.9 . . ?
C54 C54A C55 121.2(2) . . ?
C54 C54A C58A 119.7(2) . . ?
C55 C54A C58A 119.1(2) . . ?
C56 C55 C54A 121.3(3) . . ?
C56 C55 H55 119.4 . . ?
C54A C55 H55 119.4 . . ?
C55 C56 C57 120.2(2) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C58 C57 C56 120.1(3) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C58A 121.4(2) . . ?
C57 C58 H58 119.3 . . ?
C58A C58 H58 119.3 . . ?
C58 C58A C51 123.8(2) . . ?
C58 C58A C54A 117.9(2) . . ?
C51 C58A C54A 118.2(2) . . ?
C12 C11 C101 123(2) . . ?
C12 C11 Pd1 65.9(2) . . ?
C101 C11 Pd1 123.1(17) . . ?
C12 C11 H11 118.6 . . ?
C101 C11 H11 118.6 . . ?
Pd1 C11 H11 81.8 . . ?
C13 C12 C11 117.5(4) . . ?
C13 C12 Pd1 68.4(2) . . ?
C11 C12 Pd1 76.8(3) . . ?
C13 C12 H12 121.3 . . ?
C11 C12 H12 121.3 . . ?
Pd1 C12 H12 125 . . ?
C12' C13 Pd1 69.8(2) . . ?
C12 C13 Pd1 72.7(2) . . ?
C12 C13 H13A 120 . . ?
Pd1 C13 H13A 75.5 . . ?
C12 C13 H13B 120 . . ?
Pd1 C13 H13B 123.2 . . ?
H13A C13 H13B 120 . . ?
C12' C13 H13C 115.8 . . ?
C12 C13 H13C 88.5 . . ?
Pd1 C13 H13C 77.4 . . ?
C12' C13 H13D 124.2 . . ?
Pd1 C13 H13D 124 . . ?
H13C C13 H13D 120 . . ?
C12' C11' C201 127.5(7) . . ?
C12' C11' Pd1 66.6(3) . . ?
C201 C11' Pd1 125(3) . . ?
C12' C11' H11' 116.2 . . ?
C201 C11' H11' 116.2 . . ?
Pd1 C11' H11' 78.5 . . ?
C11' C12' C13 126.0(5) . . ?
C11' C12' Pd1 78.4(3) . . ?
C13 C12' Pd1 71.1(2) . . ?
C11' C12' H12' 117 . . ?
C13 C12' H12' 117 . . ?
Pd1 C12' H12' 125.3 . . ?
C106 C101 C102 118.4(10) . . ?
C106 C101 C11 118.8(9) . . ?
C102 C101 C11 122.8(9) . . ?
C101 C102 C103 120.9(10) . . ?
C101 C102 H102 119.6 . . ?
C103 C102 H102 119.6 . . ?
C104 C103 C102 121.3(8) . . ?
C104 C103 H103 119.3 . . ?
C102 C103 H103 119.3 . . ?
C103 C104 C105 119.9(7) . . ?
C103 C104 H104 120 . . ?
C105 C104 H104 120 . . ?
C104 C105 C106 118.8(8) . . ?
C104 C105 H105 120.6 . . ?
C106 C105 H105 120.6 . . ?
C101 C106 C105 120.6(8) . . ?
C101 C106 H106 119.7 . . ?
C105 C106 H106 119.7 . . ?
C206 C201 C202 119.2(10) . . ?
C206 C201 C11' 116.4(10) . . ?
C202 C201 C11' 123.0(17) . . ?
C203 C202 C201 119.7(9) . . ?
C203 C202 H202 120.1 . . ?
C201 C202 H202 120.1 . . ?
C204 C203 C202 122.2(9) . . ?
C204 C203 H203 118.9 . . ?
C202 C203 H203 118.9 . . ?
C203 C204 C205 119.0(8) . . ?
C203 C204 H204 120.5 . . ?
C205 C204 H204 120.5 . . ?
C204 C205 C206 120.0(7) . . ?
C204 C205 H205 120 . . ?
C206 C205 H205 120 . . ?
C201 C206 C205 119.7(8) . . ?
C201 C206 H206 120.1 . . ?
C205 C206 H206 120.1 . . ?

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

data_rda606o
_database_code_depnum_ccdc_archive 'CCDC 1518961'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_vrf_PLAT605_rda606o             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        38 A**3  

         
RESPONSE: Any residual electron density that may be due to solvent 
molecules was removed by use of the Program Squeeze.
;


_audit_creation_date             2016-03-15T11:27:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C42 H45 Cl N4 Pd'
_chemical_formula_moiety         'C42 H45 Cl N4 Pd'
_chemical_formula_weight         747.67
_chemical_absolute_configuration unk

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_Int_Tables_number      43
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   86.5994(8)
_cell_length_b                   25.6783(3)
_cell_length_c                   12.9003(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     28686.7(6)
_cell_formula_units_Z            32
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21809
_cell_measurement_theta_min      1.841
_cell_measurement_theta_max      30.612

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

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.072
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             12416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0371
-1 0 0 0.0354
1 -1 -2 0.2242
0 -1 0 0.1113
0 1 0 0.1219
0 -5 1 0.1499
-2 5 2 0.1654


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

_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
       CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  0.956

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

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0077591
_diffrn_orient_matrix_ub_12      -0.008674
_diffrn_orient_matrix_ub_13      -0.0031896
_diffrn_orient_matrix_ub_21      -0.0025527
_diffrn_orient_matrix_ub_22      0.0262191
_diffrn_orient_matrix_ub_23      -0.0028287
_diffrn_orient_matrix_ub_31      0.00059
_diffrn_orient_matrix_ub_32      -0.0008261
_diffrn_orient_matrix_ub_33      -0.0548118
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_number            77123
_diffrn_reflns_limit_h_min       -124
_diffrn_reflns_limit_h_max       106
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         31.414
_diffrn_reflns_theta_full        30
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_reflns_number_total             22322
_reflns_number_gt                21032
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'

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

_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
The largest peak is 0.78 Angstroms from Pd2; the deepest hole is 0.83
  Angstroms from H24D.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+258.6184P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         22322
_refine_ls_number_parameters     865
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.147
_refine_ls_wR_factor_gt          0.145
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 8117 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(14)
_refine_diff_density_max         2.095
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.116

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.66778(2) 0.93333(2) 0.55315(3) 0.02374(9) Uani 1 d . .
Pd2 Pd 0.70714(2) 0.73361(2) 1.00391(4) 0.02899(11) Uani 1 d . .
Cl1 Cl 0.69231(2) 0.94451(7) 0.47618(14) 0.0344(3) Uani 1 d . .
Cl2 Cl 0.68297(2) 0.77433(7) 1.03381(15) 0.0378(4) Uani 1 d . .
C11 C 0.67441(7) 0.8862(2) 0.6731(5) 0.0248(11) Uani 1 d . .
N12 N 0.66793(6) 0.8396(2) 0.6914(4) 0.0271(10) Uani 1 d . .
C121 C 0.65550(7) 0.8156(3) 0.6374(6) 0.0328(14) Uani 1 d . .
C122 C 0.64206(8) 0.8032(3) 0.6928(7) 0.0376(16) Uani 1 d . .
C123 C 0.63037(9) 0.7751(3) 0.6390(9) 0.049(2) Uani 1 d . .
H123 H 0.6212 0.7658 0.6744 0.059 Uiso 1 calc . .
C124 C 0.63212(11) 0.7613(3) 0.5382(10) 0.064(3) Uani 1 d . .
H124 H 0.6242 0.7418 0.5055 0.077 Uiso 1 calc . .
C125 C 0.64702(14) 0.7620(4) 0.3752(9) 0.063(3) Uani 1 d . .
H125 H 0.6391 0.743 0.3411 0.075 Uiso 1 calc . .
C126 C 0.66027(16) 0.7767(4) 0.3186(8) 0.070(3) Uani 1 d . .
H126 H 0.6611 0.7693 0.2467 0.084 Uiso 1 calc . .
C127 C 0.67195(12) 0.8024(3) 0.3710(7) 0.048(2) Uani 1 d . .
H127 H 0.681 0.8119 0.3342 0.058 Uiso 1 calc . .
C128 C 0.67087(9) 0.8146(3) 0.4739(6) 0.0382(16) Uani 1 d . .
H128 H 0.6793 0.8313 0.5074 0.046 Uiso 1 calc . .
C129 C 0.64522(10) 0.7746(3) 0.4807(8) 0.051(2) Uani 1 d . .
C120 C 0.65748(9) 0.8027(3) 0.5308(6) 0.0389(18) Uani 1 d . .
N131 N 0.64043(7) 0.8144(3) 0.7992(7) 0.0414(14) Uani 1 d . .
C132 C 0.64097(9) 0.8701(3) 0.8302(7) 0.0424(18) Uani 1 d . .
H13A H 0.6307 0.8863 0.8186 0.051 Uiso 1 calc . .
H13B H 0.6486 0.8888 0.7869 0.051 Uiso 1 calc . .
C133 C 0.64534(12) 0.8749(4) 0.9429(7) 0.055(2) Uani 1 d . .
H13C H 0.6448 0.9119 0.9641 0.065 Uiso 1 calc . .
H13D H 0.6561 0.8627 0.9527 0.065 Uiso 1 calc . .
C134 C 0.63443(13) 0.8424(5) 1.0118(10) 0.071(3) Uani 1 d . .
H13E H 0.6383 0.8422 1.0839 0.085 Uiso 1 calc . .
H13F H 0.624 0.8584 1.0119 0.085 Uiso 1 calc . .
C135 C 0.63341(12) 0.7874(5) 0.9719(9) 0.066(3) Uani 1 d . .
H13G H 0.6435 0.77 0.9806 0.079 Uiso 1 calc . .
H13H H 0.6257 0.7679 1.013 0.079 Uiso 1 calc . .
C136 C 0.62895(10) 0.7864(4) 0.8609(10) 0.061(3) Uani 1 d . .
H13I H 0.6282 0.7499 0.8367 0.073 Uiso 1 calc . .
H13J H 0.6187 0.8028 0.8521 0.073 Uiso 1 calc . .
C13 C 0.67632(7) 0.8094(3) 0.7725(6) 0.0322(14) Uani 1 d . .
H13K H 0.6824 0.7805 0.7416 0.039 Uiso 1 calc . .
H13L H 0.6691 0.7951 0.8249 0.039 Uiso 1 calc . .
C14 C 0.68679(7) 0.8505(3) 0.8187(6) 0.0319(13) Uani 1 d . .
H14A H 0.6829 0.8624 0.887 0.038 Uiso 1 calc . .
H14B H 0.6975 0.8375 0.8264 0.038 Uiso 1 calc . .
N15 N 0.68588(6) 0.8922(2) 0.7409(4) 0.0284(11) Uani 1 d . .
C151 C 0.69582(8) 0.9371(3) 0.7536(5) 0.0322(13) Uani 1 d . .
C152 C 0.71150(8) 0.9309(4) 0.7383(6) 0.0421(18) Uani 1 d . .
C153 C 0.72101(10) 0.9756(5) 0.7614(8) 0.059(3) Uani 1 d . .
H153 H 0.7317 0.974 0.745 0.07 Uiso 1 calc . .
C154 C 0.71553(12) 1.0189(4) 0.8045(8) 0.061(3) Uani 1 d . .
H154 H 0.7224 1.0463 0.8212 0.073 Uiso 1 calc . .
C155 C 0.69369(16) 1.0694(4) 0.8742(7) 0.062(3) Uani 1 d . .
H155 H 0.7005 1.0968 0.8935 0.074 Uiso 1 calc . .
C156 C 0.67821(15) 1.0741(3) 0.8938(7) 0.059(3) Uani 1 d . .
H156 H 0.6743 1.1042 0.9275 0.071 Uiso 1 calc . .
C157 C 0.66812(12) 1.0336(3) 0.8632(7) 0.048(2) Uani 1 d . .
H157 H 0.6573 1.0372 0.8749 0.058 Uiso 1 calc . .
C158 C 0.67358(9) 0.9895(3) 0.8172(5) 0.0341(14) Uani 1 d . .
H158 H 0.6665 0.9626 0.7992 0.041 Uiso 1 calc . .
C159 C 0.69964(11) 1.0248(3) 0.8260(6) 0.045(2) Uani 1 d . .
C150 C 0.68955(9) 0.9826(3) 0.7957(5) 0.0349(15) Uani 1 d . .
N141 N 0.71809(7) 0.8834(3) 0.7086(6) 0.0468(17) Uani 1 d . .
C142 C 0.71302(9) 0.8557(4) 0.6163(7) 0.047(2) Uani 1 d . .
H14C H 0.7018 0.8615 0.6059 0.056 Uiso 1 calc . .
H14D H 0.7185 0.8696 0.555 0.056 Uiso 1 calc . .
C143 C 0.71593(12) 0.8018(4) 0.6252(11) 0.066(3) Uani 1 d . .
H14E H 0.7119 0.7832 0.5637 0.08 Uiso 1 calc . .
H14F H 0.7107 0.7877 0.6876 0.08 Uiso 1 calc . .
C144 C 0.73361(12) 0.7936(5) 0.6339(11) 0.070(3) Uani 1 d . .
H14G H 0.7359 0.7564 0.6473 0.084 Uiso 1 calc . .
H14H H 0.7387 0.8038 0.5682 0.084 Uiso 1 calc . .
C145 C 0.73970(14) 0.8271(5) 0.7231(10) 0.075(3) Uani 1 d . .
H14I H 0.7363 0.8116 0.7894 0.09 Uiso 1 calc . .
H14J H 0.7511 0.8262 0.722 0.09 Uiso 1 calc . .
C146 C 0.73492(10) 0.8789(6) 0.7199(10) 0.072(3) Uani 1 d . .
H14K H 0.74 0.8966 0.661 0.086 Uiso 1 calc . .
H14L H 0.7382 0.8966 0.7845 0.086 Uiso 1 calc . .
C111 C 0.65494(8) 0.9817(3) 0.4334(5) 0.0300(13) Uani 1 d . .
H111 H 0.6585 1.0102 0.4738 0.036 Uiso 1 calc . .
C112 C 0.64578(8) 0.9440(3) 0.4806(6) 0.0345(15) Uani 1 d . .
H112 H 0.6405 0.9193 0.439 0.041 Uiso 1 calc . .
C113 C 0.64426(8) 0.9418(3) 0.5898(6) 0.0337(15) Uani 1 d . .
H11A H 0.6495 0.9664 0.632 0.04 Uiso 1 calc . .
H11B H 0.638 0.9159 0.6208 0.04 Uiso 1 calc . .
C101 C 0.65930(8) 0.9792(3) 0.3246(5) 0.0327(14) Uani 1 d . .
C102 C 0.66245(9) 1.0251(3) 0.2704(7) 0.0402(17) Uani 1 d . .
H102 H 0.6618 1.0576 0.3052 0.048 Uiso 1 calc . .
C103 C 0.66653(11) 1.0238(4) 0.1668(7) 0.050(2) Uani 1 d . .
H103 H 0.6683 1.0555 0.1306 0.06 Uiso 1 calc . .
C104 C 0.66806(13) 0.9769(4) 0.1153(7) 0.058(2) Uani 1 d . .
H104 H 0.671 0.9765 0.0443 0.07 Uiso 1 calc . .
C105 C 0.66537(13) 0.9308(4) 0.1670(7) 0.055(2) Uani 1 d . .
H105 H 0.6665 0.8984 0.1321 0.066 Uiso 1 calc . .
C106 C 0.66100(10) 0.9321(3) 0.2709(6) 0.0433(18) Uani 1 d . .
H106 H 0.6591 0.9003 0.3063 0.052 Uiso 1 calc . .
C21 C 0.70020(7) 0.6570(3) 1.0077(6) 0.0308(13) Uani 1 d . .
N22 N 0.70718(6) 0.6209(2) 1.0680(5) 0.0314(12) Uani 1 d . .
C221 C 0.72101(7) 0.6274(3) 1.1266(6) 0.0327(14) Uani 1 d . .
C222 C 0.73401(8) 0.5974(3) 1.1007(6) 0.0357(15) Uani 1 d . .
C223 C 0.74749(8) 0.6041(4) 1.1631(8) 0.047(2) Uani 1 d . .
H223 H 0.7564 0.5841 1.1477 0.057 Uiso 1 calc . .
C224 C 0.74798(9) 0.6375(4) 1.2425(9) 0.056(2) Uani 1 d . .
H224 H 0.7573 0.6414 1.2805 0.067 Uiso 1 calc . .
C225 C 0.73533(14) 0.6998(6) 1.3533(12) 0.090(5) Uani 1 d . .
H225 H 0.7446 0.7034 1.3922 0.108 Uiso 1 calc . .
C226 C 0.72282(15) 0.7277(7) 1.3815(12) 0.097(5) Uani 1 d . .
H226 H 0.7234 0.7507 1.4391 0.116 Uiso 1 calc . .
C227 C 0.70874(12) 0.7231(4) 1.3257(9) 0.059(2) Uani 1 d . .
H227 H 0.6999 0.7427 1.3459 0.07 Uiso 1 calc . .
C228 C 0.70799(8) 0.6905(3) 1.2438(6) 0.0380(15) Uani 1 d . .
H228 H 0.6986 0.6871 1.2065 0.046 Uiso 1 calc . .
C229 C 0.73511(10) 0.6666(4) 1.2706(8) 0.052(2) Uani 1 d . .
C220 C 0.72123(8) 0.6610(3) 1.2124(6) 0.0373(16) Uani 1 d . .
N231 N 0.73347(7) 0.5615(3) 1.0203(6) 0.0446(16) Uani 1 d . .
C232 C 0.73166(10) 0.5817(4) 0.9142(8) 0.049(2) Uani 1 d . .
H23A H 0.7418 0.5943 0.8884 0.059 Uiso 1 calc . .
H23B H 0.7244 0.6115 0.9147 0.059 Uiso 1 calc . .
C233 C 0.72571(12) 0.5408(5) 0.8437(9) 0.062(3) Uani 1 d . .
H23C H 0.7253 0.5545 0.772 0.075 Uiso 1 calc . .
H23D H 0.7151 0.5312 0.8645 0.075 Uiso 1 calc . .
C234 C 0.73600(11) 0.4924(5) 0.8467(11) 0.071(3) Uani 1 d . .
H23E H 0.7311 0.4641 0.8064 0.085 Uiso 1 calc . .
H23F H 0.746 0.5005 0.8137 0.085 Uiso 1 calc . .
C235 C 0.73869(12) 0.4744(4) 0.9535(10) 0.063(3) Uani 1 d . .
H23G H 0.7464 0.4459 0.9528 0.076 Uiso 1 calc . .
H23H H 0.7289 0.4604 0.9823 0.076 Uiso 1 calc . .
C236 C 0.74447(10) 0.5180(4) 1.0221(8) 0.052(2) Uani 1 d . .
H23I H 0.7457 0.5051 1.094 0.063 Uiso 1 calc . .
H23J H 0.7547 0.53 0.9974 0.063 Uiso 1 calc . .
C23 C 0.69844(8) 0.5713(3) 1.0731(6) 0.0344(15) Uani 1 d . .
H23K H 0.6932 0.5673 1.1409 0.041 Uiso 1 calc . .
H23L H 0.7053 0.541 1.0612 0.041 Uiso 1 calc . .
C24 C 0.68688(8) 0.5775(3) 0.9863(6) 0.0318(14) Uani 1 d . .
H24A H 0.6898 0.5564 0.925 0.038 Uiso 1 calc . .
H24B H 0.6763 0.5676 1.0088 0.038 Uiso 1 calc . .
N25 N 0.68800(7) 0.6343(2) 0.9642(5) 0.0341(13) Uani 1 d . .
C251 C 0.67780(9) 0.6550(3) 0.8892(6) 0.0349(15) Uani 1 d . .
C252 C 0.66221(10) 0.6571(3) 0.9092(7) 0.0396(17) Uani 1 d . .
C253 C 0.65199(10) 0.6711(3) 0.8261(9) 0.053(3) Uani 1 d . .
H253 H 0.6413 0.6747 0.8396 0.063 Uiso 1 calc . .
C254 C 0.65737(14) 0.6796(3) 0.7283(9) 0.063(3) Uani 1 d . .
H254 H 0.6502 0.6877 0.6749 0.076 Uiso 1 calc . .
C255 C 0.67905(17) 0.6847(3) 0.6031(7) 0.065(3) Uani 1 d . .
H255 H 0.6722 0.6947 0.5493 0.078 Uiso 1 calc . .
C256 C 0.69419(19) 0.6787(4) 0.5809(8) 0.074(4) Uani 1 d . .
H256 H 0.6978 0.683 0.512 0.088 Uiso 1 calc . .
C257 C 0.70441(15) 0.6659(4) 0.6607(9) 0.064(3) Uani 1 d . .
H257 H 0.7151 0.6617 0.6457 0.076 Uiso 1 calc . .
C258 C 0.69926(12) 0.6592(3) 0.7606(7) 0.050(2) Uani 1 d . .
H258 H 0.7065 0.6511 0.8137 0.06 Uiso 1 calc . .
C259 C 0.67317(13) 0.6766(3) 0.7037(7) 0.050(2) Uani 1 d . .
C250 C 0.68353(10) 0.6643(3) 0.7856(6) 0.0386(17) Uani 1 d . .
N241 N 0.65608(7) 0.6426(2) 1.0087(7) 0.0408(14) Uani 1 d . .
C242 C 0.66131(8) 0.6721(3) 1.0978(7) 0.0404(17) Uani 1 d . .
H24C H 0.6555 0.7053 1.1018 0.048 Uiso 1 calc . .
H24D H 0.6724 0.6805 1.0897 0.048 Uiso 1 calc . .
C243 C 0.65894(9) 0.6418(3) 1.1957(9) 0.050(2) Uani 1 d . .
H24E H 0.6624 0.6627 1.2559 0.06 Uiso 1 calc . .
H24F H 0.6651 0.6094 1.1936 0.06 Uiso 1 calc . .
C244 C 0.64171(10) 0.6284(4) 1.2071(10) 0.062(3) Uani 1 d . .
H24G H 0.6402 0.6056 1.2682 0.074 Uiso 1 calc . .
H24H H 0.6357 0.6607 1.2176 0.074 Uiso 1 calc . .
C245 C 0.63620(10) 0.6005(4) 1.1091(12) 0.071(4) Uani 1 d . .
H24I H 0.6413 0.5661 1.1048 0.086 Uiso 1 calc . .
H24J H 0.6249 0.5947 1.114 0.086 Uiso 1 calc . .
C246 C 0.63960(8) 0.6304(3) 1.0127(11) 0.061(3) Uani 1 d . .
H24K H 0.6367 0.6096 0.9512 0.073 Uiso 1 calc . .
H24L H 0.6335 0.6631 1.0119 0.073 Uiso 1 calc . .
C211 C 0.71985(8) 0.8100(3) 0.9974(6) 0.0345(14) Uani 1 d . .
H211 H 0.7165 0.8098 0.9272 0.041 Uiso 1 calc . .
C212 C 0.72918(8) 0.7690(3) 1.0302(6) 0.0394(17) Uani 1 d . .
H212 H 0.7344 0.7712 1.0948 0.047 Uiso 1 calc . .
C213 C 0.73089(8) 0.7239(3) 0.9673(7) 0.0382(16) Uani 1 d . .
H21A H 0.7257 0.7216 0.9027 0.046 Uiso 1 calc . .
H21B H 0.7373 0.696 0.9898 0.046 Uiso 1 calc . .
C201 C 0.71475(8) 0.8535(3) 1.0627(7) 0.0381(15) Uani 1 d . .
C202 C 0.71259(9) 0.9031(3) 1.0227(6) 0.0394(16) Uani 1 d . .
H202 H 0.7144 0.9085 0.9509 0.047 Uiso 1 calc . .
C203 C 0.70799(11) 0.9446(4) 1.0820(8) 0.053(2) Uani 1 d . .
H203 H 0.7066 0.9779 1.0513 0.063 Uiso 1 calc . .
C204 C 0.70545(11) 0.9378(4) 1.1849(8) 0.054(2) Uani 1 d . .
H204 H 0.7023 0.9664 1.2262 0.065 Uiso 1 calc . .
C205 C 0.70747(10) 0.8890(4) 1.2302(8) 0.0499(19) Uani 1 d . .
H205 H 0.7057 0.8843 1.3023 0.06 Uiso 1 calc . .
C206 C 0.71200(9) 0.8483(3) 1.1706(7) 0.0425(17) Uani 1 d . .
H206 H 0.7134 0.8152 1.202 0.051 Uiso 1 calc . .



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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C11 2.047(7) . ?
Pd1 C113 2.102(7) . ?
Pd1 C112 2.140(6) . ?
Pd1 C111 2.273(6) . ?
Pd1 Cl1 2.3628(16) . ?
Pd2 C21 2.058(7) . ?
Pd2 C213 2.125(7) . ?
Pd2 C212 2.141(7) . ?
Pd2 C211 2.251(6) . ?
Pd2 Cl2 2.3717(18) . ?
C11 N15 1.333(8) . ?
C11 N12 1.340(8) . ?
N12 C121 1.423(8) . ?
N12 C13 1.492(9) . ?
C121 C122 1.402(11) . ?
C121 C120 1.425(12) . ?
C122 N131 1.408(13) . ?
C122 C123 1.425(11) . ?
C123 C124 1.356(16) . ?
C123 H123 0.95 . ?
C124 C129 1.397(16) . ?
C124 H124 0.95 . ?
C125 C129 1.409(15) . ?
C125 C126 1.412(18) . ?
C125 H125 0.95 . ?
C126 C127 1.384(15) . ?
C126 H126 0.95 . ?
C127 C128 1.367(12) . ?
C127 H127 0.95 . ?
C128 C120 1.406(12) . ?
C128 H128 0.95 . ?
C129 C120 1.437(10) . ?
N131 C136 1.463(11) . ?
N131 C132 1.485(11) . ?
C132 C133 1.508(13) . ?
C132 H13A 0.99 . ?
C132 H13B 0.99 . ?
C133 C134 1.541(14) . ?
C133 H13C 0.99 . ?
C133 H13D 0.99 . ?
C134 C135 1.505(18) . ?
C134 H13E 0.99 . ?
C134 H13F 0.99 . ?
C135 C136 1.483(18) . ?
C135 H13G 0.99 . ?
C135 H13H 0.99 . ?
C136 H13I 0.99 . ?
C136 H13J 0.99 . ?
C13 C14 1.514(9) . ?
C13 H13K 0.99 . ?
C13 H13L 0.99 . ?
C14 N15 1.470(9) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
N15 C151 1.448(8) . ?
C151 C152 1.382(10) . ?
C151 C150 1.399(11) . ?
C152 N141 1.401(12) . ?
C152 C153 1.443(12) . ?
C153 C154 1.331(16) . ?
C153 H153 0.95 . ?
C154 C159 1.411(14) . ?
C154 H154 0.95 . ?
C155 C156 1.369(17) . ?
C155 C159 1.402(14) . ?
C155 H155 0.95 . ?
C156 C157 1.414(13) . ?
C156 H156 0.95 . ?
C157 C158 1.364(11) . ?
C157 H157 0.95 . ?
C158 C150 1.421(11) . ?
C158 H158 0.95 . ?
C159 C150 1.446(10) . ?
N141 C142 1.454(11) . ?
N141 C146 1.469(11) . ?
C142 C143 1.412(15) . ?
C142 H14C 0.99 . ?
C142 H14D 0.99 . ?
C143 C144 1.549(15) . ?
C143 H14E 0.99 . ?
C143 H14F 0.99 . ?
C144 C145 1.531(19) . ?
C144 H14G 0.99 . ?
C144 H14H 0.99 . ?
C145 C146 1.392(18) . ?
C145 H14I 0.99 . ?
C145 H14J 0.99 . ?
C146 H14K 0.99 . ?
C146 H14L 0.99 . ?
C111 C112 1.393(10) . ?
C111 C101 1.455(10) . ?
C111 H111 0.95 . ?
C112 C113 1.415(12) . ?
C112 H112 0.95 . ?
C113 H11A 0.95 . ?
C113 H11B 0.95 . ?
C101 C102 1.397(11) . ?
C101 C106 1.401(11) . ?
C102 C103 1.383(13) . ?
C102 H102 0.95 . ?
C103 C104 1.381(15) . ?
C103 H103 0.95 . ?
C104 C105 1.379(15) . ?
C104 H104 0.95 . ?
C105 C106 1.393(13) . ?
C105 H105 0.95 . ?
C106 H106 0.95 . ?
C21 N25 1.330(8) . ?
C21 N22 1.352(9) . ?
N22 C221 1.426(9) . ?
N22 C23 1.484(9) . ?
C221 C220 1.403(12) . ?
C221 C222 1.404(10) . ?
C222 N231 1.389(11) . ?
C222 C223 1.429(11) . ?
C223 C224 1.336(15) . ?
C223 H223 0.95 . ?
C224 C229 1.391(14) . ?
C224 H224 0.95 . ?
C225 C226 1.349(19) . ?
C225 C229 1.365(16) . ?
C225 H225 0.95 . ?
C226 C227 1.421(15) . ?
C226 H226 0.95 . ?
C227 C228 1.350(13) . ?
C227 H227 0.95 . ?
C228 C220 1.433(11) . ?
C228 H228 0.95 . ?
C229 C220 1.425(11) . ?
N231 C236 1.469(11) . ?
N231 C232 1.472(12) . ?
C232 C233 1.481(15) . ?
C232 H23A 0.99 . ?
C232 H23B 0.99 . ?
C233 C234 1.529(16) . ?
C233 H23C 0.99 . ?
C233 H23D 0.99 . ?
C234 C235 1.471(19) . ?
C234 H23E 0.99 . ?
C234 H23F 0.99 . ?
C235 C236 1.512(16) . ?
C235 H23G 0.99 . ?
C235 H23H 0.99 . ?
C236 H23I 0.99 . ?
C236 H23J 0.99 . ?
C23 C24 1.511(10) . ?
C23 H23K 0.99 . ?
C23 H23L 0.99 . ?
C24 N25 1.491(9) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
N25 C251 1.413(9) . ?
C251 C252 1.376(12) . ?
C251 C250 1.446(12) . ?
C252 C253 1.436(11) . ?
C252 N241 1.438(12) . ?
C253 C254 1.362(17) . ?
C253 H253 0.95 . ?
C254 C259 1.406(16) . ?
C254 H254 0.95 . ?
C255 C256 1.351(19) . ?
C255 C259 1.410(16) . ?
C255 H255 0.95 . ?
C256 C257 1.397(17) . ?
C256 H256 0.95 . ?
C257 C258 1.375(15) . ?
C257 H257 0.95 . ?
C258 C250 1.406(13) . ?
C258 H258 0.95 . ?
C259 C250 1.421(11) . ?
N241 C242 1.449(12) . ?
N241 C246 1.462(9) . ?
C242 C243 1.497(13) . ?
C242 H24C 0.99 . ?
C242 H24D 0.99 . ?
C243 C244 1.538(12) . ?
C243 H24E 0.99 . ?
C243 H24F 0.99 . ?
C244 C245 1.529(18) . ?
C244 H24G 0.99 . ?
C244 H24H 0.99 . ?
C245 C246 1.491(19) . ?
C245 H24I 0.99 . ?
C245 H24J 0.99 . ?
C246 H24K 0.99 . ?
C246 H24L 0.99 . ?
C211 C212 1.393(11) . ?
C211 C201 1.468(12) . ?
C211 H211 0.95 . ?
C212 C213 1.424(12) . ?
C212 H212 0.95 . ?
C213 H21A 0.95 . ?
C213 H21B 0.95 . ?
C201 C202 1.386(11) . ?
C201 C206 1.418(13) . ?
C202 C203 1.371(13) . ?
C202 H202 0.95 . ?
C203 C204 1.356(15) . ?
C203 H203 0.95 . ?
C204 C205 1.394(14) . ?
C204 H204 0.95 . ?
C205 C206 1.356(13) . ?
C205 H205 0.95 . ?
C206 H206 0.95 . ?

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
C11 Pd1 C113 99.4(3) . . ?
C11 Pd1 C112 131.0(3) . . ?
C113 Pd1 C112 39.0(3) . . ?
C11 Pd1 C111 167.0(2) . . ?
C113 Pd1 C111 67.8(3) . . ?
C112 Pd1 C111 36.6(3) . . ?
C11 Pd1 Cl1 97.88(18) . . ?
C113 Pd1 Cl1 162.4(2) . . ?
C112 Pd1 Cl1 127.0(2) . . ?
C111 Pd1 Cl1 95.03(18) . . ?
C21 Pd2 C213 100.1(3) . . ?
C21 Pd2 C212 131.5(3) . . ?
C213 Pd2 C212 39.0(3) . . ?
C21 Pd2 C211 167.7(3) . . ?
C213 Pd2 C211 67.7(3) . . ?
C212 Pd2 C211 36.9(3) . . ?
C21 Pd2 Cl2 99.20(18) . . ?
C213 Pd2 Cl2 160.5(2) . . ?
C212 Pd2 Cl2 125.0(2) . . ?
C211 Pd2 Cl2 93.06(19) . . ?
N15 C11 N12 107.5(6) . . ?
N15 C11 Pd1 129.5(5) . . ?
N12 C11 Pd1 122.9(4) . . ?
C11 N12 C121 128.1(6) . . ?
C11 N12 C13 112.6(5) . . ?
C121 N12 C13 119.0(5) . . ?
C122 C121 N12 118.5(7) . . ?
C122 C121 C120 122.7(6) . . ?
N12 C121 C120 118.8(7) . . ?
C121 C122 N131 122.3(7) . . ?
C121 C122 C123 117.1(8) . . ?
N131 C122 C123 120.5(8) . . ?
C124 C123 C122 121.4(9) . . ?
C124 C123 H123 119.3 . . ?
C122 C123 H123 119.3 . . ?
C123 C124 C129 122.3(7) . . ?
C123 C124 H124 118.8 . . ?
C129 C124 H124 118.8 . . ?
C129 C125 C126 121.8(9) . . ?
C129 C125 H125 119.1 . . ?
C126 C125 H125 119.1 . . ?
C127 C126 C125 118.0(9) . . ?
C127 C126 H126 121 . . ?
C125 C126 H126 121 . . ?
C128 C127 C126 122.2(11) . . ?
C128 C127 H127 118.9 . . ?
C126 C127 H127 118.9 . . ?
C127 C128 C120 120.9(8) . . ?
C127 C128 H128 119.5 . . ?
C120 C128 H128 119.5 . . ?
C124 C129 C125 123.1(9) . . ?
C124 C129 C120 119.0(9) . . ?
C125 C129 C120 117.9(10) . . ?
C128 C120 C121 123.6(6) . . ?
C128 C120 C129 118.9(8) . . ?
C121 C120 C129 117.5(8) . . ?
C122 N131 C136 119.8(8) . . ?
C122 N131 C132 117.1(6) . . ?
C136 N131 C132 110.4(7) . . ?
N131 C132 C133 110.2(7) . . ?
N131 C132 H13A 109.6 . . ?
C133 C132 H13A 109.6 . . ?
N131 C132 H13B 109.6 . . ?
C133 C132 H13B 109.6 . . ?
H13A C132 H13B 108.1 . . ?
C132 C133 C134 111.0(9) . . ?
C132 C133 H13C 109.4 . . ?
C134 C133 H13C 109.4 . . ?
C132 C133 H13D 109.4 . . ?
C134 C133 H13D 109.4 . . ?
H13C C133 H13D 108 . . ?
C135 C134 C133 110.3(9) . . ?
C135 C134 H13E 109.6 . . ?
C133 C134 H13E 109.6 . . ?
C135 C134 H13F 109.6 . . ?
C133 C134 H13F 109.6 . . ?
H13E C134 H13F 108.1 . . ?
C136 C135 C134 111.2(9) . . ?
C136 C135 H13G 109.4 . . ?
C134 C135 H13G 109.4 . . ?
C136 C135 H13H 109.4 . . ?
C134 C135 H13H 109.4 . . ?
H13G C135 H13H 108 . . ?
N131 C136 C135 109.9(9) . . ?
N131 C136 H13I 109.7 . . ?
C135 C136 H13I 109.7 . . ?
N131 C136 H13J 109.7 . . ?
C135 C136 H13J 109.7 . . ?
H13I C136 H13J 108.2 . . ?
N12 C13 C14 101.8(5) . . ?
N12 C13 H13K 111.4 . . ?
C14 C13 H13K 111.4 . . ?
N12 C13 H13L 111.4 . . ?
C14 C13 H13L 111.4 . . ?
H13K C13 H13L 109.3 . . ?
N15 C14 C13 102.0(5) . . ?
N15 C14 H14A 111.4 . . ?
C13 C14 H14A 111.4 . . ?
N15 C14 H14B 111.4 . . ?
C13 C14 H14B 111.4 . . ?
H14A C14 H14B 109.2 . . ?
C11 N15 C151 127.6(6) . . ?
C11 N15 C14 113.8(5) . . ?
C151 N15 C14 118.1(5) . . ?
C152 C151 C150 122.2(6) . . ?
C152 C151 N15 118.5(7) . . ?
C150 C151 N15 118.6(6) . . ?
C151 C152 N141 122.6(7) . . ?
C151 C152 C153 116.1(9) . . ?
N141 C152 C153 121.1(8) . . ?
C154 C153 C152 123.1(8) . . ?
C154 C153 H153 118.4 . . ?
C152 C153 H153 118.4 . . ?
C153 C154 C159 121.3(7) . . ?
C153 C154 H154 119.3 . . ?
C159 C154 H154 119.3 . . ?
C156 C155 C159 120.9(8) . . ?
C156 C155 H155 119.5 . . ?
C159 C155 H155 119.5 . . ?
C155 C156 C157 119.3(9) . . ?
C155 C156 H156 120.4 . . ?
C157 C156 H156 120.4 . . ?
C158 C157 C156 121.2(10) . . ?
C158 C157 H157 119.4 . . ?
C156 C157 H157 119.4 . . ?
C157 C158 C150 121.7(7) . . ?
C157 C158 H158 119.1 . . ?
C150 C158 H158 119.1 . . ?
C155 C159 C154 122.2(8) . . ?
C155 C159 C150 120.6(9) . . ?
C154 C159 C150 117.1(8) . . ?
C151 C150 C158 123.9(6) . . ?
C151 C150 C159 119.7(7) . . ?
C158 C150 C159 116.3(7) . . ?
C152 N141 C142 121.8(7) . . ?
C152 N141 C146 116.4(8) . . ?
C142 N141 C146 110.0(8) . . ?
C143 C142 N141 111.0(9) . . ?
C143 C142 H14C 109.4 . . ?
N141 C142 H14C 109.4 . . ?
C143 C142 H14D 109.4 . . ?
N141 C142 H14D 109.4 . . ?
H14C C142 H14D 108 . . ?
C142 C143 C144 108.3(9) . . ?
C142 C143 H14E 110 . . ?
C144 C143 H14E 110 . . ?
C142 C143 H14F 110 . . ?
C144 C143 H14F 110 . . ?
H14E C143 H14F 108.4 . . ?
C145 C144 C143 108.6(10) . . ?
C145 C144 H14G 110 . . ?
C143 C144 H14G 110 . . ?
C145 C144 H14H 110 . . ?
C143 C144 H14H 110 . . ?
H14G C144 H14H 108.4 . . ?
C146 C145 C144 114.3(10) . . ?
C146 C145 H14I 108.7 . . ?
C144 C145 H14I 108.7 . . ?
C146 C145 H14J 108.7 . . ?
C144 C145 H14J 108.7 . . ?
H14I C145 H14J 107.6 . . ?
C145 C146 N141 111.9(11) . . ?
C145 C146 H14K 109.2 . . ?
N141 C146 H14K 109.2 . . ?
C145 C146 H14L 109.2 . . ?
N141 C146 H14L 109.2 . . ?
H14K C146 H14L 107.9 . . ?
C112 C111 C101 122.6(7) . . ?
C112 C111 Pd1 66.5(4) . . ?
C101 C111 Pd1 120.3(5) . . ?
C112 C111 H111 118.7 . . ?
C101 C111 H111 118.7 . . ?
Pd1 C111 H111 83.7 . . ?
C111 C112 C113 121.0(7) . . ?
C111 C112 Pd1 76.9(4) . . ?
C113 C112 Pd1 69.1(4) . . ?
C111 C112 H112 119.5 . . ?
C113 C112 H112 119.5 . . ?
Pd1 C112 H112 126.4 . . ?
C112 C113 Pd1 72.0(4) . . ?
C112 C113 H11A 120 . . ?
Pd1 C113 H11A 74.5 . . ?
C112 C113 H11B 120 . . ?
Pd1 C113 H11B 125.3 . . ?
H11A C113 H11B 120 . . ?
C102 C101 C106 117.4(7) . . ?
C102 C101 C111 119.7(7) . . ?
C106 C101 C111 122.8(7) . . ?
C103 C102 C101 120.9(8) . . ?
C103 C102 H102 119.6 . . ?
C101 C102 H102 119.6 . . ?
C104 C103 C102 120.6(9) . . ?
C104 C103 H103 119.7 . . ?
C102 C103 H103 119.7 . . ?
C105 C104 C103 120.0(9) . . ?
C105 C104 H104 120 . . ?
C103 C104 H104 120 . . ?
C104 C105 C106 119.4(8) . . ?
C104 C105 H105 120.3 . . ?
C106 C105 H105 120.3 . . ?
C105 C106 C101 121.7(8) . . ?
C105 C106 H106 119.2 . . ?
C101 C106 H106 119.2 . . ?
N25 C21 N22 107.4(6) . . ?
N25 C21 Pd2 129.8(5) . . ?
N22 C21 Pd2 122.5(5) . . ?
C21 N22 C221 126.9(6) . . ?
C21 N22 C23 112.7(5) . . ?
C221 N22 C23 120.3(6) . . ?
C220 C221 C222 120.9(7) . . ?
C220 C221 N22 120.1(6) . . ?
C222 C221 N22 118.9(7) . . ?
N231 C222 C221 121.0(7) . . ?
N231 C222 C223 121.9(7) . . ?
C221 C222 C223 117.0(8) . . ?
C224 C223 C222 122.4(8) . . ?
C224 C223 H223 118.8 . . ?
C222 C223 H223 118.8 . . ?
C223 C224 C229 121.3(8) . . ?
C223 C224 H224 119.3 . . ?
C229 C224 H224 119.3 . . ?
C226 C225 C229 122.1(11) . . ?
C226 C225 H225 118.9 . . ?
C229 C225 H225 118.9 . . ?
C225 C226 C227 120.5(11) . . ?
C225 C226 H226 119.7 . . ?
C227 C226 H226 119.7 . . ?
C228 C227 C226 119.3(10) . . ?
C228 C227 H227 120.3 . . ?
C226 C227 H227 120.3 . . ?
C227 C228 C220 120.7(8) . . ?
C227 C228 H228 119.6 . . ?
C220 C228 H228 119.6 . . ?
C225 C229 C224 121.9(9) . . ?
C225 C229 C220 119.2(10) . . ?
C224 C229 C220 118.9(9) . . ?
C221 C220 C229 119.3(8) . . ?
C221 C220 C228 122.5(7) . . ?
C229 C220 C228 118.2(8) . . ?
C222 N231 C236 118.1(8) . . ?
C222 N231 C232 117.6(7) . . ?
C236 N231 C232 110.6(7) . . ?
N231 C232 C233 111.0(8) . . ?
N231 C232 H23A 109.4 . . ?
C233 C232 H23A 109.4 . . ?
N231 C232 H23B 109.4 . . ?
C233 C232 H23B 109.4 . . ?
H23A C232 H23B 108 . . ?
C232 C233 C234 111.0(9) . . ?
C232 C233 H23C 109.4 . . ?
C234 C233 H23C 109.4 . . ?
C232 C233 H23D 109.4 . . ?
C234 C233 H23D 109.4 . . ?
H23C C233 H23D 108 . . ?
C235 C234 C233 111.8(9) . . ?
C235 C234 H23E 109.3 . . ?
C233 C234 H23E 109.3 . . ?
C235 C234 H23F 109.3 . . ?
C233 C234 H23F 109.3 . . ?
H23E C234 H23F 107.9 . . ?
C234 C235 C236 111.6(9) . . ?
C234 C235 H23G 109.3 . . ?
C236 C235 H23G 109.3 . . ?
C234 C235 H23H 109.3 . . ?
C236 C235 H23H 109.3 . . ?
H23G C235 H23H 108 . . ?
N231 C236 C235 109.8(8) . . ?
N231 C236 H23I 109.7 . . ?
C235 C236 H23I 109.7 . . ?
N231 C236 H23J 109.7 . . ?
C235 C236 H23J 109.7 . . ?
H23I C236 H23J 108.2 . . ?
N22 C23 C24 102.4(5) . . ?
N22 C23 H23K 111.3 . . ?
C24 C23 H23K 111.3 . . ?
N22 C23 H23L 111.3 . . ?
C24 C23 H23L 111.3 . . ?
H23K C23 H23L 109.2 . . ?
N25 C24 C23 101.6(5) . . ?
N25 C24 H24A 111.4 . . ?
C23 C24 H24A 111.4 . . ?
N25 C24 H24B 111.4 . . ?
C23 C24 H24B 111.4 . . ?
H24A C24 H24B 109.3 . . ?
C21 N25 C251 128.4(6) . . ?
C21 N25 C24 113.5(6) . . ?
C251 N25 C24 117.3(6) . . ?
C252 C251 N25 120.0(7) . . ?
C252 C251 C250 120.2(7) . . ?
N25 C251 C250 118.7(7) . . ?
C251 C252 C253 118.3(9) . . ?
C251 C252 N241 121.3(7) . . ?
C253 C252 N241 120.3(8) . . ?
C254 C253 C252 121.4(9) . . ?
C254 C253 H253 119.3 . . ?
C252 C253 H253 119.3 . . ?
C253 C254 C259 122.2(8) . . ?
C253 C254 H254 118.9 . . ?
C259 C254 H254 118.9 . . ?
C256 C255 C259 121.9(10) . . ?
C256 C255 H255 119 . . ?
C259 C255 H255 119 . . ?
C255 C256 C257 119.1(11) . . ?
C255 C256 H256 120.5 . . ?
C257 C256 H256 120.5 . . ?
C258 C257 C256 121.0(12) . . ?
C258 C257 H257 119.5 . . ?
C256 C257 H257 119.5 . . ?
C257 C258 C250 121.2(9) . . ?
C257 C258 H258 119.4 . . ?
C250 C258 H258 119.4 . . ?
C254 C259 C255 123.4(9) . . ?
C254 C259 C250 117.3(9) . . ?
C255 C259 C250 119.3(10) . . ?
C258 C250 C259 117.5(8) . . ?
C258 C250 C251 121.9(7) . . ?
C259 C250 C251 120.5(8) . . ?
C252 N241 C242 117.2(6) . . ?
C252 N241 C246 116.5(8) . . ?
C242 N241 C246 112.9(8) . . ?
N241 C242 C243 110.8(7) . . ?
N241 C242 H24C 109.5 . . ?
C243 C242 H24C 109.5 . . ?
N241 C242 H24D 109.5 . . ?
C243 C242 H24D 109.5 . . ?
H24C C242 H24D 108.1 . . ?
C242 C243 C244 109.3(8) . . ?
C242 C243 H24E 109.8 . . ?
C244 C243 H24E 109.8 . . ?
C242 C243 H24F 109.8 . . ?
C244 C243 H24F 109.8 . . ?
H24E C243 H24F 108.3 . . ?
C245 C244 C243 109.2(8) . . ?
C245 C244 H24G 109.8 . . ?
C243 C244 H24G 109.8 . . ?
C245 C244 H24H 109.8 . . ?
C243 C244 H24H 109.8 . . ?
H24G C244 H24H 108.3 . . ?
C246 C245 C244 112.8(8) . . ?
C246 C245 H24I 109 . . ?
C244 C245 H24I 109 . . ?
C246 C245 H24J 109 . . ?
C244 C245 H24J 109 . . ?
H24I C245 H24J 107.8 . . ?
N241 C246 C245 109.4(9) . . ?
N241 C246 H24K 109.8 . . ?
C245 C246 H24K 109.8 . . ?
N241 C246 H24L 109.8 . . ?
C245 C246 H24L 109.8 . . ?
H24K C246 H24L 108.3 . . ?
C212 C211 C201 125.1(7) . . ?
C212 C211 Pd2 67.3(4) . . ?
C201 C211 Pd2 119.7(5) . . ?
C212 C211 H211 117.5 . . ?
C201 C211 H211 117.5 . . ?
Pd2 C211 H211 83.2 . . ?
C211 C212 C213 120.1(7) . . ?
C211 C212 Pd2 75.8(4) . . ?
C213 C212 Pd2 69.9(4) . . ?
C211 C212 H212 119.9 . . ?
C213 C212 H212 119.9 . . ?
Pd2 C212 H212 126.1 . . ?
C212 C213 Pd2 71.1(4) . . ?
C212 C213 H21A 120 . . ?
Pd2 C213 H21A 75 . . ?
C212 C213 H21B 120 . . ?
Pd2 C213 H21B 125.6 . . ?
H21A C213 H21B 120 . . ?
C202 C201 C206 115.5(8) . . ?
C202 C201 C211 121.7(8) . . ?
C206 C201 C211 122.8(7) . . ?
C203 C202 C201 123.0(8) . . ?
C203 C202 H202 118.5 . . ?
C201 C202 H202 118.5 . . ?
C204 C203 C202 119.5(9) . . ?
C204 C203 H203 120.2 . . ?
C202 C203 H203 120.2 . . ?
C203 C204 C205 120.4(9) . . ?
C203 C204 H204 119.8 . . ?
C205 C204 H204 119.8 . . ?
C206 C205 C204 119.4(9) . . ?
C206 C205 H205 120.3 . . ?
C204 C205 H205 120.3 . . ?
C205 C206 C201 122.2(8) . . ?
C205 C206 H206 118.9 . . ?
C201 C206 H206 118.9 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.146 0.635 -0.023 23.8 3.0
2 0.229 0.589 0.042 37.7 6.2
3 0.271 0.911 0.042 37.2 6.3
4 0.354 0.865 -0.023 23.8 2.9
5 0.646 0.135 -0.023 23.8 3.0
6 0.729 0.089 0.042 37.7 6.2
7 0.771 0.411 0.042 37.2 6.3
8 0.854 0.365 -0.023 23.8 2.9
9 0.198 0.552 0.154 6.6 0.0
10 0.302 0.948 0.154 7.2 0.0
11 0.698 0.052 0.154 6.6 0.0
12 0.802 0.448 0.154 7.2 0.0
13 0.104 0.885 0.227 23.8 4.0
14 0.396 0.615 0.227 23.7 4.2
15 0.604 0.385 0.227 23.8 4.0
16 0.896 0.115 0.227 23.7 4.2
17 0.021 0.839 0.292 37.2 4.6
18 0.479 0.661 0.292 37.6 4.2
19 0.521 0.339 0.292 37.2 4.6
20 0.979 0.161 0.292 37.6 4.2
21 0.052 0.802 0.404 7.1 0.2
22 0.448 0.698 0.404 6.7 0.1
23 0.552 0.302 0.404 7.1 0.2
24 0.948 0.198 0.404 6.7 0.1
25 0.146 0.135 0.477 23.8 3.0
26 0.354 0.365 0.477 23.8 2.9
27 0.646 0.635 0.477 23.8 3.0
28 0.854 0.865 0.477 23.8 2.9
29 0.229 0.089 0.542 37.7 6.2
30 0.271 0.411 0.542 37.2 6.3
31 0.729 0.589 0.542 37.7 6.2
32 0.771 0.911 0.542 37.2 6.3
33 0.198 0.052 0.654 6.6 0.0
34 0.302 0.448 0.654 7.2 0.0
35 0.698 0.552 0.654 6.6 0.0
36 0.802 0.948 0.654 7.2 0.0
37 0.104 0.385 0.727 23.8 4.0
38 0.396 0.115 0.727 23.7 4.2
39 0.604 0.885 0.727 23.8 4.0
40 0.896 0.615 0.727 23.7 4.2
41 0.021 0.339 0.792 37.2 4.6
42 0.479 0.161 0.792 37.6 4.2
43 0.521 0.839 0.792 37.2 4.6
44 0.979 0.661 0.792 37.6 4.2
45 0.052 0.302 0.904 7.1 0.2
46 0.448 0.198 0.904 6.7 0.1
47 0.552 0.802 0.904 7.1 0.2
48 0.948 0.698 0.904 6.7 0.1

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

data_rda080
_database_code_depnum_ccdc_archive 'CCDC 1518962'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT973_rda080              
;
PROBLEM: Check Calcd Positive Residual Density on     Ru2       2.33 eA-3  

RESPONSE: This could not be modelled as it is too close
          to the atom (0.93 A) and no twinnig was observed.
;

# end Validation Reply Form

_audit_creation_date             2012-10-10T11:22:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C58 H75 Cl6 N4 O2 P Ru'
_chemical_formula_moiety         'C56 H71 Cl2 N4 O2 P Ru, 2(C H2 Cl2)'
_chemical_formula_weight         1204.96

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-p 2yn'
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                   21.7830(7)
_cell_length_b                   12.5026(5)
_cell_length_c                   42.0112(16)
_cell_angle_alpha                90
_cell_angle_beta                 99.268(4)
_cell_angle_gamma                90
_cell_volume                     11292.1(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18224
_cell_measurement_theta_min      3.1868
_cell_measurement_theta_max      68.4966

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

_exptl_crystal_description       fragment
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5024
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 -3 0.0308
0 -2 3 0.0435
3 0 -1 0.0512
0 0 -1 0.0369
-1 0 -2 0.0609
2 0 3 0.055
-1 0 1 0.0668
-1 0 9 0.0202

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    5.482
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
      CrysAlisPro, Oxford Diffraction Ltd.,
Analytical numeric absorption correction using a multifaceted crystal
                  model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)


;
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_T_max  0.777

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      0.0483652
_diffrn_orient_matrix_ub_12      -0.0222073
_diffrn_orient_matrix_ub_13      0.0302465
_diffrn_orient_matrix_ub_21      0.0409135
_diffrn_orient_matrix_ub_22      -0.0600212
_diffrn_orient_matrix_ub_23      -0.0208379
_diffrn_orient_matrix_ub_31      0.0334456
_diffrn_orient_matrix_ub_32      0.1052739
_diffrn_orient_matrix_ub_33      -0.005455
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_number            105688
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         68.67
_diffrn_reflns_theta_full        68
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.97
_reflns_number_total             20207
_reflns_number_gt                14265
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(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.

Each of the four dichloromethane solvent molecules were modelled as being
disordered over two sets of sites.  The occupancies of molecules 1 and 2 
were refined to 0.726(6) and its complement  with those for molecules 3 
and 4 constrained to 0.5 after trial refinement. Geometries of the
disordered atoms were restrained to ideal values.
;
_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)+(0.1195P)²+6.9926P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         20207
_refine_ls_number_parameters     1377
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.2221
_refine_ls_wR_factor_gt          0.1872
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.134

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.790641(18) 0.74490(4) 0.507113(10) 0.03310(14) Uani 1 1 d . . .
Ru2 Ru 0.507504(18) 0.98267(4) 0.274143(9) 0.02734(13) Uani 1 1 d . . .
Cl1 Cl 0.88403(6) 0.75422(11) 0.48509(3) 0.0325(3) Uani 1 1 d . . .
Cl2 Cl 0.68941(6) 0.70073(17) 0.51863(4) 0.0516(4) Uani 1 1 d . . .
Cl3 Cl 0.59061(7) 0.98596(12) 0.24398(3) 0.0402(3) Uani 1 1 d . . .
Cl4 Cl 0.43889(6) 1.01550(12) 0.31245(3) 0.0367(3) Uani 1 1 d . . .
C1 C 0.7468(2) 0.8679(6) 0.47804(13) 0.0356(14) Uani 1 1 d . . .
N2 N 0.7134(2) 0.8484(4) 0.44836(11) 0.0365(11) Uani 1 1 d . . .
C21 C 0.7159(3) 0.7546(5) 0.42960(13) 0.0380(15) Uani 1 1 d . . .
C22 C 0.7637(3) 0.7393(6) 0.41144(14) 0.0413(16) Uani 1 1 d . . .
C23 C 0.7640(3) 0.6461(6) 0.39301(15) 0.0452(16) Uani 1 1 d . . .
H23 H 0.7981 0.6334 0.382 0.054 Uiso 1 1 calc R . .
C24 C 0.7169(3) 0.5729(6) 0.39027(14) 0.0432(15) Uani 1 1 d . . .
H24 H 0.7184 0.5109 0.3774 0.052 Uiso 1 1 calc R . .
C24A C 0.6659(3) 0.5893(6) 0.40668(13) 0.0384(14) Uani 1 1 d . . .
C25 C 0.6149(3) 0.5161(6) 0.40334(15) 0.0451(16) Uani 1 1 d . . .
H25 H 0.6154 0.4549 0.39 0.054 Uiso 1 1 calc R . .
C26 C 0.5656(3) 0.5327(6) 0.41905(16) 0.0493(17) Uani 1 1 d . . .
H26 H 0.5316 0.4843 0.4164 0.059 Uiso 1 1 calc R . .
C27 C 0.5658(3) 0.6228(6) 0.43938(15) 0.0479(17) Uani 1 1 d . . .
H27 H 0.5315 0.6339 0.4504 0.057 Uiso 1 1 calc R . .
C28 C 0.6137(3) 0.6944(6) 0.44368(14) 0.0394(14) Uani 1 1 d . . .
H28 H 0.6127 0.7539 0.4577 0.047 Uiso 1 1 calc R . .
C28A C 0.6651(3) 0.6794(5) 0.42708(13) 0.0377(14) Uani 1 1 d . . .
N241 N 0.8096(2) 0.8199(5) 0.41113(11) 0.0406(13) Uani 1 1 d . . .
C242 C 0.8702(3) 0.7828(6) 0.40468(15) 0.0460(16) Uani 1 1 d . . .
H24A H 0.8667 0.7578 0.3821 0.055 Uiso 1 1 calc R . .
H24B H 0.8851 0.7225 0.4192 0.055 Uiso 1 1 calc R . .
C243 C 0.9150(3) 0.8746(6) 0.41041(15) 0.0448(16) Uani 1 1 d . . .
H24C H 0.9178 0.8992 0.433 0.054 Uiso 1 1 calc R . .
H24D H 0.9568 0.8501 0.4073 0.054 Uiso 1 1 calc R . .
O244 O 0.8962(2) 0.9625(5) 0.38906(11) 0.0539(13) Uani 1 1 d . . .
C245 C 0.8372(3) 0.9992(7) 0.39395(18) 0.057(2) Uani 1 1 d . . .
H24E H 0.8235 1.0576 0.3785 0.069 Uiso 1 1 calc R . .
H24F H 0.8404 1.0288 0.416 0.069 Uiso 1 1 calc R . .
C246 C 0.7886(3) 0.9101(6) 0.38955(17) 0.0488(17) Uani 1 1 d . . .
H24G H 0.7486 0.9378 0.3945 0.059 Uiso 1 1 calc R . .
H24H H 0.7819 0.8853 0.3669 0.059 Uiso 1 1 calc R . .
C3 C 0.6696(3) 0.9357(5) 0.43823(15) 0.0391(14) Uani 1 1 d . . .
H3A H 0.6275 0.9189 0.4428 0.047 Uiso 1 1 calc R . .
H3B H 0.6671 0.9514 0.415 0.047 Uiso 1 1 calc R . .
C4 C 0.6983(3) 1.0267(6) 0.45854(14) 0.0398(14) Uani 1 1 d . . .
H4A H 0.7247 1.0714 0.4468 0.048 Uiso 1 1 calc R . .
H4B H 0.6662 1.0721 0.4661 0.048 Uiso 1 1 calc R . .
N5 N 0.7359(2) 0.9684(5) 0.48562(11) 0.0376(12) Uani 1 1 d . . .
C51 C 0.7674(3) 1.0312(5) 0.51186(13) 0.0343(13) Uani 1 1 d . . .
C52 C 0.7324(3) 1.0789(6) 0.53298(15) 0.0430(15) Uani 1 1 d . . .
C53 C 0.7636(3) 1.1443(6) 0.55788(14) 0.0439(16) Uani 1 1 d . . .
H53 H 0.741 1.1737 0.5733 0.053 Uiso 1 1 calc R . .
C54 C 0.8251(3) 1.1660(6) 0.56023(15) 0.0427(15) Uani 1 1 d . . .
H54 H 0.8452 1.2067 0.578 0.051 Uiso 1 1 calc R . .
C54A C 0.8601(3) 1.1291(5) 0.53670(14) 0.0364(13) Uani 1 1 d . . .
C55 C 0.9225(3) 1.1601(6) 0.53698(15) 0.0440(15) Uani 1 1 d . . .
H55 H 0.943 1.2029 0.5542 0.053 Uiso 1 1 calc R . .
C56 C 0.9538(3) 1.1293(5) 0.51282(16) 0.0394(14) Uani 1 1 d . . .
H56 H 0.9949 1.1541 0.5124 0.047 Uiso 1 1 calc R . .
C57 C 0.9242(3) 1.0602(6) 0.48854(15) 0.0407(14) Uani 1 1 d . . .
H57 H 0.9463 1.0372 0.472 0.049 Uiso 1 1 calc R . .
C58 C 0.8645(3) 1.0255(5) 0.48817(14) 0.0348(13) Uani 1 1 d . . .
H58 H 0.8461 0.9781 0.4717 0.042 Uiso 1 1 calc R . .
C58A C 0.8301(3) 1.0593(5) 0.51202(13) 0.0346(13) Uani 1 1 d . . .
N541 N 0.6666(2) 1.0626(6) 0.52918(13) 0.0511(15) Uani 1 1 d . . .
C542 C 0.6463(3) 0.9556(7) 0.53669(17) 0.056(2) Uani 1 1 d . . .
H54A H 0.6554 0.9436 0.5603 0.067 Uiso 1 1 calc R . .
H54B H 0.6693 0.9015 0.5261 0.067 Uiso 1 1 calc R . .
C543 C 0.5780(3) 0.9434(8) 0.5252(2) 0.065(2) Uani 1 1 d . . .
H54C H 0.5696 0.9489 0.5014 0.078 Uiso 1 1 calc R . .
H54D H 0.5645 0.8716 0.5313 0.078 Uiso 1 1 calc R . .
O544 O 0.5428(2) 1.0232(6) 0.53884(14) 0.0776(19) Uani 1 1 d . . .
C545 C 0.5620(3) 1.1241(9) 0.5303(2) 0.076(3) Uani 1 1 d . . .
H54E H 0.5367 1.1795 0.539 0.091 Uiso 1 1 calc R . .
H54F H 0.5549 1.1306 0.5065 0.091 Uiso 1 1 calc R . .
C546 C 0.6313(3) 1.1437(8) 0.54335(19) 0.064(2) Uani 1 1 d . . .
H54G H 0.6437 1.2161 0.5373 0.076 Uiso 1 1 calc R . .
H54H H 0.6391 1.1379 0.5672 0.076 Uiso 1 1 calc R . .
C200 C 0.8042(3) 0.8252(5) 0.54433(13) 0.0349(13) Uani 1 1 d . . .
H200 H 0.7668 0.8382 0.5526 0.042 Uiso 1 1 calc R . .
C201 C 0.8582(3) 0.8743(6) 0.56443(13) 0.0375(14) Uani 1 1 d . . .
C202 C 0.9195(3) 0.8710(6) 0.55784(13) 0.0399(14) Uani 1 1 d . . .
H202 H 0.9281 0.837 0.5388 0.048 Uiso 1 1 calc R . .
C203 C 0.9673(3) 0.9176(6) 0.57927(14) 0.0413(15) Uani 1 1 d . . .
H203 H 1.0086 0.9154 0.5746 0.05 Uiso 1 1 calc R . .
C204 C 0.9560(3) 0.9671(6) 0.60707(15) 0.0449(16) Uani 1 1 d . . .
H204 H 0.9893 0.9979 0.6215 0.054 Uiso 1 1 calc R . .
C205 C 0.8961(3) 0.9716(6) 0.61378(14) 0.0472(16) Uani 1 1 d . . .
H205 H 0.8881 1.0058 0.6329 0.057 Uiso 1 1 calc R . .
C206 C 0.8474(3) 0.9262(6) 0.59255(14) 0.0398(14) Uani 1 1 d . . .
H206 H 0.8062 0.9305 0.5972 0.048 Uiso 1 1 calc R . .
P1 P 0.82400(6) 0.57300(13) 0.53152(3) 0.0321(3) Uani 1 1 d . . .
C111 C 0.9107(2) 0.5549(5) 0.54195(13) 0.0322(12) Uani 1 1 d . . .
H111 H 0.9285 0.5957 0.5251 0.039 Uiso 1 1 calc R . .
C112 C 0.9370(3) 0.6088(5) 0.57404(14) 0.0357(13) Uani 1 1 d . . .
H11A H 0.9246 0.5676 0.5921 0.043 Uiso 1 1 calc R . .
H11B H 0.9196 0.6818 0.5746 0.043 Uiso 1 1 calc R . .
C113 C 1.0083(3) 0.6149(5) 0.57813(15) 0.0400(14) Uani 1 1 d . . .
H11C H 1.0207 0.6594 0.5607 0.048 Uiso 1 1 calc R . .
H11D H 1.0248 0.6488 0.5991 0.048 Uiso 1 1 calc R . .
C114 C 1.0355(3) 0.5027(6) 0.57686(14) 0.0400(15) Uani 1 1 d . . .
H11E H 1.0812 0.5078 0.578 0.048 Uiso 1 1 calc R . .
H11F H 1.027 0.461 0.5957 0.048 Uiso 1 1 calc R . .
C115 C 1.0078(3) 0.4452(6) 0.54605(14) 0.0400(14) Uani 1 1 d . . .
H11G H 1.024 0.3711 0.5468 0.048 Uiso 1 1 calc R . .
H11H H 1.0213 0.4817 0.5274 0.048 Uiso 1 1 calc R . .
C116 C 0.9369(3) 0.4418(5) 0.54101(14) 0.0375(13) Uani 1 1 d . . .
H11I H 0.923 0.3978 0.5581 0.045 Uiso 1 1 calc R . .
H11J H 0.921 0.4083 0.5199 0.045 Uiso 1 1 calc R . .
C121 C 0.7870(3) 0.5357(6) 0.56668(13) 0.0385(14) Uani 1 1 d . . .
H121 H 0.7417 0.5289 0.5579 0.046 Uiso 1 1 calc R . .
C122 C 0.7902(3) 0.6201(6) 0.59293(15) 0.0434(15) Uani 1 1 d . . .
H12A H 0.7733 0.6886 0.5834 0.052 Uiso 1 1 calc R . .
H12B H 0.8341 0.6318 0.6029 0.052 Uiso 1 1 calc R . .
C123 C 0.7522(3) 0.5831(6) 0.61886(15) 0.0456(16) Uani 1 1 d . . .
H12C H 0.7554 0.638 0.6361 0.055 Uiso 1 1 calc R . .
H12D H 0.7079 0.577 0.609 0.055 Uiso 1 1 calc R . .
C124 C 0.7741(3) 0.4774(6) 0.63367(15) 0.0476(17) Uani 1 1 d . . .
H12E H 0.7477 0.4562 0.6497 0.057 Uiso 1 1 calc R . .
H12F H 0.8175 0.4841 0.6449 0.057 Uiso 1 1 calc R . .
C125 C 0.7705(3) 0.3917(6) 0.60734(15) 0.0458(16) Uani 1 1 d . . .
H12G H 0.7879 0.3238 0.617 0.055 Uiso 1 1 calc R . .
H12H H 0.7264 0.379 0.598 0.055 Uiso 1 1 calc R . .
C126 C 0.8062(3) 0.4251(5) 0.58061(14) 0.0396(14) Uani 1 1 d . . .
H12I H 0.7991 0.3715 0.5631 0.048 Uiso 1 1 calc R . .
H12J H 0.8513 0.4258 0.5892 0.048 Uiso 1 1 calc R . .
C131 C 0.8018(3) 0.4599(5) 0.50316(13) 0.0370(14) Uani 1 1 d . . .
H131 H 0.8238 0.3954 0.5134 0.044 Uiso 1 1 calc R . .
C132 C 0.7331(3) 0.4314(6) 0.49627(15) 0.0488(18) Uani 1 1 d . . .
H13A H 0.7096 0.4894 0.4837 0.059 Uiso 1 1 calc R . .
H13B H 0.7168 0.4233 0.5168 0.059 Uiso 1 1 calc R . .
C133 C 0.7243(4) 0.3244(7) 0.47677(16) 0.058(2) Uani 1 1 d . . .
H13C H 0.7456 0.2656 0.49 0.069 Uiso 1 1 calc R . .
H13D H 0.6795 0.3068 0.4717 0.069 Uiso 1 1 calc R . .
C134 C 0.7511(3) 0.3345(6) 0.44557(15) 0.0479(17) Uani 1 1 d . . .
H13E H 0.7482 0.2645 0.4345 0.057 Uiso 1 1 calc R . .
H13F H 0.726 0.3866 0.4312 0.057 Uiso 1 1 calc R . .
C135 C 0.8185(3) 0.3710(6) 0.45161(16) 0.0463(16) Uani 1 1 d . . .
H13G H 0.8331 0.382 0.4307 0.056 Uiso 1 1 calc R . .
H13H H 0.8446 0.3148 0.4636 0.056 Uiso 1 1 calc R . .
C136 C 0.8253(3) 0.4757(5) 0.47106(14) 0.0394(14) Uani 1 1 d . . .
H13I H 0.8695 0.4977 0.4752 0.047 Uiso 1 1 calc R . .
H13J H 0.801 0.5331 0.4585 0.047 Uiso 1 1 calc R . .
C6 C 0.5532(2) 0.8592(5) 0.30249(12) 0.0296(12) Uani 1 1 d . . .
N7 N 0.6008(2) 0.8774(4) 0.32670(11) 0.0311(10) Uani 1 1 d . . .
C71 C 0.6283(3) 0.9790(5) 0.33709(13) 0.0353(13) Uani 1 1 d . . .
C72 C 0.6820(3) 1.0169(6) 0.32669(14) 0.0403(15) Uani 1 1 d . . .
C73 C 0.7072(3) 1.1156(6) 0.34091(15) 0.0420(15) Uani 1 1 d . . .
H73 H 0.7431 1.1446 0.3339 0.05 Uiso 1 1 calc RD . .
C74 C 0.6827(3) 1.1684(6) 0.36351(16) 0.0451(15) Uani 1 1 d . . .
H74 H 0.7012 1.2336 0.3718 0.054 Uiso 1 1 calc R . .
C74A C 0.6295(3) 1.1292(5) 0.37552(14) 0.0399(14) Uani 1 1 d . . .
C75 C 0.6043(3) 1.1808(7) 0.40028(16) 0.0533(18) Uani 1 1 d . . .
H75 H 0.622 1.2461 0.4089 0.064 Uiso 1 1 calc R . .
C76 C 0.5553(3) 1.1391(7) 0.41211(16) 0.0525(18) Uani 1 1 d . . .
H76 H 0.5401 1.1728 0.4296 0.063 Uiso 1 1 calc R . .
C77 C 0.5272(3) 1.0456(7) 0.39827(15) 0.0496(17) Uani 1 1 d . . .
H77 H 0.4922 1.0168 0.4062 0.06 Uiso 1 1 calc R . .
C78 C 0.5490(3) 0.9955(6) 0.37380(14) 0.0409(15) Uani 1 1 d . . .
H78 H 0.5287 0.9328 0.3647 0.049 Uiso 1 1 calc R . .
C78A C 0.6020(3) 1.0350(5) 0.36137(13) 0.0361(13) Uani 1 1 d . . .
N741 N 0.7176(2) 0.9667(5) 0.30640(13) 0.0442(13) Uani 1 1 d . . .
C742 C 0.7099(3) 0.8558(6) 0.29706(17) 0.0490(17) Uani 1 1 d . . .
H74A H 0.6746 0.8494 0.2791 0.059 Uiso 1 1 calc R . .
H74B H 0.6996 0.8139 0.3155 0.059 Uiso 1 1 calc R . .
C743 C 0.7679(4) 0.8088(8) 0.2865(2) 0.073(2) Uani 1 1 d . . .
H74C H 0.8023 0.8078 0.305 0.088 Uiso 1 1 calc R . .
H74D H 0.7596 0.7342 0.2792 0.088 Uiso 1 1 calc R . .
O744 O 0.7858(3) 0.8704(5) 0.26107(16) 0.0790(19) Uani 1 1 d . . .
C745 C 0.7992(5) 0.9766(9) 0.2723(3) 0.086(3) Uani 1 1 d . . .
H74E H 0.8142 1.0192 0.2552 0.104 Uiso 1 1 calc R . .
H74F H 0.8325 0.9752 0.2913 0.104 Uiso 1 1 calc R . .
C746 C 0.7423(4) 1.0279(7) 0.28122(19) 0.059(2) Uani 1 1 d . . .
H74G H 0.7526 1.1014 0.2891 0.071 Uiso 1 1 calc RD . .
H74H H 0.7099 1.0331 0.2618 0.071 Uiso 1 1 calc R . .
C8 C 0.6140(3) 0.7846(5) 0.34780(13) 0.0366(13) Uani 1 1 d . . .
H8A H 0.5955 0.7926 0.3677 0.044 Uiso 1 1 calc R . .
H8B H 0.6594 0.7724 0.3537 0.044 Uiso 1 1 calc R . .
C9 C 0.5830(3) 0.6956(5) 0.32669(14) 0.0360(13) Uani 1 1 d . . .
H9A H 0.6137 0.6547 0.3166 0.043 Uiso 1 1 calc R . .
H9B H 0.5605 0.6461 0.3391 0.043 Uiso 1 1 calc R . .
N10 N 0.5399(2) 0.7548(4) 0.30250(11) 0.0325(11) Uani 1 1 d . . .
C101 C 0.5008(3) 0.6941(4) 0.27858(13) 0.0311(12) Uani 1 1 d . . .
C102 C 0.4477(3) 0.6442(5) 0.28694(14) 0.0355(13) Uani 1 1 d . . .
C103 C 0.4116(3) 0.5796(5) 0.26290(17) 0.0444(15) Uani 1 1 d . . .
H103 H 0.3736 0.5496 0.2671 0.053 Uiso 1 1 calc R . .
C104 C 0.4301(3) 0.5601(6) 0.23419(16) 0.0460(16) Uani 1 1 d . . .
H104 H 0.4046 0.5173 0.2187 0.055 Uiso 1 1 calc R . .
C14A C 0.4857(3) 0.6009(5) 0.22664(15) 0.0413(14) Uani 1 1 d . . .
C105 C 0.5068(4) 0.5742(6) 0.19691(15) 0.0506(17) Uani 1 1 d . . .
H105 H 0.4823 0.5291 0.1817 0.061 Uiso 1 1 calc R . .
C106 C 0.5620(4) 0.6136(6) 0.19056(16) 0.0527(18) Uani 1 1 d . . .
H106 H 0.5761 0.596 0.171 0.063 Uiso 1 1 calc R . .
C107 C 0.5978(4) 0.6805(6) 0.21330(16) 0.0491(16) Uani 1 1 d . . .
H107 H 0.6363 0.7077 0.2088 0.059 Uiso 1 1 calc R . .
C108 C 0.5786(3) 0.7070(5) 0.24153(14) 0.0402(14) Uani 1 1 d . . .
H108 H 0.6042 0.7515 0.2565 0.048 Uiso 1 1 calc R . .
C18A C 0.5211(3) 0.6695(5) 0.24916(14) 0.0375(13) Uani 1 1 d . . .
N141 N 0.4333(2) 0.6499(4) 0.31800(12) 0.0394(12) Uani 1 1 d . . .
C142 C 0.4194(3) 0.7535(6) 0.33070(17) 0.0485(17) Uani 1 1 d . . .
H14A H 0.3764 0.7746 0.3215 0.058 Uiso 1 1 calc R . .
H14B H 0.4481 0.808 0.3244 0.058 Uiso 1 1 calc R . .
C143 C 0.4261(3) 0.7487(7) 0.36717(18) 0.0548(19) Uani 1 1 d . . .
H14C H 0.4697 0.7316 0.3764 0.066 Uiso 1 1 calc R . .
H14D H 0.4158 0.8193 0.3756 0.066 Uiso 1 1 calc R . .
O144 O 0.3856(2) 0.6688(5) 0.37680(13) 0.0666(15) Uani 1 1 d . . .
C145 C 0.3989(3) 0.5674(7) 0.36378(18) 0.0562(19) Uani 1 1 d . . .
H14E H 0.3704 0.513 0.3703 0.067 Uiso 1 1 calc R . .
H14F H 0.4419 0.5462 0.3729 0.067 Uiso 1 1 calc R . .
C146 C 0.3921(3) 0.5693(6) 0.32787(17) 0.0488(17) Uani 1 1 d . . .
H14G H 0.4026 0.4982 0.3199 0.059 Uiso 1 1 calc R . .
H14H H 0.3485 0.5858 0.3185 0.059 Uiso 1 1 calc R . .
C400 C 0.4468(3) 0.9013(5) 0.25075(15) 0.0391(14) Uani 1 1 d . . .
H400 H 0.4153 0.8822 0.263 0.047 Uiso 1 1 calc R . .
C401 C 0.4343(4) 0.8582(5) 0.21815(16) 0.0493(17) Uani 1 1 d . . .
C402 C 0.4753(4) 0.8624(6) 0.19588(16) 0.059(2) Uani 1 1 d . . .
H402 H 0.5146 0.8958 0.2019 0.071 Uiso 1 1 calc R . .
C403 C 0.4604(7) 0.8194(7) 0.16523(19) 0.093(4) Uani 1 1 d . . .
H403 H 0.4891 0.8239 0.1505 0.112 Uiso 1 1 calc R . .
C404 C 0.4039(6) 0.7702(9) 0.1562(3) 0.095(3) Uani 1 1 d U . .
H404 H 0.3943 0.7391 0.1354 0.114 Uiso 1 1 calc R . .
C405 C 0.3619(6) 0.7656(8) 0.1766(3) 0.092(3) Uani 1 1 d U . .
H405 H 0.3223 0.7341 0.1697 0.11 Uiso 1 1 calc R . .
C406 C 0.3764(4) 0.8069(6) 0.2081(2) 0.069(2) Uani 1 1 d . . .
H406 H 0.3474 0.8005 0.2226 0.083 Uiso 1 1 calc R . .
P2 P 0.47000(6) 1.15235(12) 0.24991(3) 0.0291(3) Uani 1 1 d . . .
C211 C 0.4869(3) 1.1728(5) 0.20802(12) 0.0322(12) Uani 1 1 d . . .
H211 H 0.526 1.1317 0.2072 0.039 Uiso 1 1 calc R . .
C212 C 0.4370(3) 1.1198(5) 0.18243(14) 0.0397(14) Uani 1 1 d . . .
H21A H 0.428 1.0467 0.1895 0.048 Uiso 1 1 calc R . .
H21B H 0.398 1.1618 0.18 0.048 Uiso 1 1 calc R . .
C213 C 0.4605(3) 1.1145(5) 0.15011(14) 0.0415(14) Uani 1 1 d . . .
H21C H 0.4979 1.0683 0.1522 0.05 Uiso 1 1 calc R . .
H21D H 0.4281 1.0824 0.1337 0.05 Uiso 1 1 calc R . .
C214 C 0.4767(4) 1.2255(6) 0.13918(15) 0.0526(18) Uani 1 1 d . . .
H21E H 0.4384 1.2691 0.1346 0.063 Uiso 1 1 calc R . .
H21F H 0.4945 1.2195 0.119 0.063 Uiso 1 1 calc R . .
C215 C 0.5233(3) 1.2810(6) 0.16482(14) 0.0471(16) Uani 1 1 d . . .
H21G H 0.5633 1.2418 0.1675 0.057 Uiso 1 1 calc R . .
H21H H 0.5309 1.3545 0.1575 0.057 Uiso 1 1 calc R . .
C216 C 0.5002(3) 1.2864(5) 0.19712(14) 0.0417(14) Uani 1 1 d . . .
H21I H 0.4619 1.33 0.195 0.05 Uiso 1 1 calc R . .
H21J H 0.5321 1.3206 0.2134 0.05 Uiso 1 1 calc R . .
C221 C 0.3869(3) 1.1834(5) 0.25110(14) 0.0362(13) Uani 1 1 d . . .
H221 H 0.3839 1.1865 0.2746 0.043 Uiso 1 1 calc R . .
C222 C 0.3413(3) 1.0955(5) 0.23760(15) 0.0383(13) Uani 1 1 d . . .
H22A H 0.3547 1.0266 0.2481 0.046 Uiso 1 1 calc R . .
H22B H 0.3415 1.0876 0.2142 0.046 Uiso 1 1 calc R . .
C223 C 0.2752(3) 1.1214(6) 0.24330(17) 0.0445(15) Uani 1 1 d . . .
H22C H 0.2462 1.0661 0.2329 0.053 Uiso 1 1 calc R . .
H22D H 0.2738 1.12 0.2667 0.053 Uiso 1 1 calc R . .
C224 C 0.2542(3) 1.2300(6) 0.22992(18) 0.0488(17) Uani 1 1 d . . .
H22E H 0.2123 1.2457 0.2351 0.059 Uiso 1 1 calc R . .
H22F H 0.251 1.229 0.2062 0.059 Uiso 1 1 calc R . .
C225 C 0.2988(3) 1.3173(6) 0.24367(17) 0.0499(17) Uani 1 1 d . . .
H22G H 0.2982 1.324 0.2671 0.06 Uiso 1 1 calc R . .
H22H H 0.2849 1.3863 0.2334 0.06 Uiso 1 1 calc R . .
C226 C 0.3658(3) 1.2937(6) 0.23814(16) 0.0423(14) Uani 1 1 d . . .
H22I H 0.3677 1.297 0.2148 0.051 Uiso 1 1 calc R . .
H22J H 0.3943 1.3488 0.2491 0.051 Uiso 1 1 calc R . .
C231 C 0.5126(3) 1.2671(5) 0.27208(13) 0.0330(13) Uani 1 1 d . . .
H231 H 0.5014 1.3326 0.2588 0.04 Uiso 1 1 calc R . .
C232 C 0.4955(3) 1.2886(5) 0.30551(14) 0.0356(13) Uani 1 1 d . . .
H23A H 0.5084 1.2272 0.3199 0.043 Uiso 1 1 calc R . .
H23B H 0.4499 1.2971 0.3037 0.043 Uiso 1 1 calc R . .
C233 C 0.5282(3) 1.3906(5) 0.31974(15) 0.0409(14) Uani 1 1 d . . .
H23C H 0.512 1.4526 0.3063 0.049 Uiso 1 1 calc R . .
H23D H 0.5184 1.4022 0.3417 0.049 Uiso 1 1 calc R . .
C234 C 0.5979(3) 1.3843(5) 0.32139(14) 0.0379(13) Uani 1 1 d . . .
H23E H 0.6151 1.3308 0.3378 0.046 Uiso 1 1 calc R . .
H23F H 0.6166 1.4545 0.3281 0.046 Uiso 1 1 calc R . .
C235 C 0.6153(3) 1.3530(6) 0.28878(16) 0.0437(15) Uani 1 1 d . . .
H23G H 0.6046 1.4124 0.2733 0.052 Uiso 1 1 calc R . .
H23H H 0.6609 1.3416 0.2913 0.052 Uiso 1 1 calc R . .
C236 C 0.5828(3) 1.2536(6) 0.27528(15) 0.0401(15) Uani 1 1 d . . .
H23I H 0.5963 1.1924 0.2897 0.048 Uiso 1 1 calc R . .
H23J H 0.5941 1.2381 0.2539 0.048 Uiso 1 1 calc R . .
Cl11 Cl 0.31595(18) -0.0184(4) 0.37457(8) 0.1090(18) Uani 0.726(6) 1 d PD A 1
Cl12 Cl 0.2134(5) 0.0114(6) 0.3224(2) 0.111(2) Uani 0.726(6) 1 d PD A 1
C10 C 0.2892(4) -0.0291(10) 0.3347(2) 0.059(3) Uani 0.726(6) 1 d PD A 1
H10A H 0.2929 -0.1047 0.3283 0.071 Uiso 0.726(6) 1 calc PR A 1
H10B H 0.3165 0.0138 0.3229 0.071 Uiso 0.726(6) 1 calc PR A 1
Cl13 Cl 0.2754(5) -0.1373(11) 0.3590(2) 0.110(4) Uani 0.274(6) 1 d PD A 2
Cl14 Cl 0.2202(15) 0.0436(17) 0.3259(7) 0.111(2) Uani 0.274(6) 1 d PD A 2
C10' C 0.2133(7) -0.0906(16) 0.3368(5) 0.057(7) Uani 0.274(6) 1 d PDU A 2
H10C H 0.1778 -0.0977 0.3486 0.068 Uiso 0.274(6) 1 calc PRD A 2
H10D H 0.204 -0.1343 0.3169 0.068 Uiso 0.274(6) 1 calc PRD A 2
Cl21 Cl 0.6783(3) 0.8467(3) 0.15214(12) 0.0730(11) Uani 0.726(6) 1 d PD A 1
Cl22 Cl 0.7281(3) 1.0360(4) 0.18666(10) 0.1108(18) Uani 0.726(6) 1 d PD A 1
C20 C 0.6946(7) 0.9104(10) 0.1898(3) 0.081(5) Uani 0.726(6) 1 d PD A 1
H20A H 0.6556 0.9186 0.1989 0.097 Uiso 0.726(6) 1 calc PR A 1
H20B H 0.7233 0.8653 0.2048 0.097 Uiso 0.726(6) 1 calc PR A 1
Cl23 Cl 0.6628(14) 0.8484(19) 0.1480(6) 0.218(17) Uani 0.274(6) 1 d PD A 2
Cl24 Cl 0.6706(13) 1.0583(10) 0.1766(5) 0.173(11) Uani 0.274(6) 1 d PD A 2
C20' C 0.670(3) 0.9208(18) 0.1840(7) 0.081(5) Uani 0.274(6) 1 d PD A 2
H20C H 0.635 0.9031 0.1954 0.097 Uiso 0.274(6) 1 calc PR A 2
H20D H 0.7092 0.9001 0.1981 0.097 Uiso 0.274(6) 1 calc PR A 2
Cl31 Cl 0.34555(10) 0.2594(2) 0.33710(6) 0.0823(7) Uani 0.5 1 d PD B 1
Cl32 Cl 0.3890(3) 0.2436(8) 0.40423(11) 0.133(4) Uani 0.5 1 d PD B 1
C30 C 0.4067(4) 0.2220(9) 0.36721(18) 0.079(3) Uani 0.5 1 d PD B 1
H30A H 0.4161 0.1452 0.3648 0.095 Uiso 0.5 1 calc PR B 1
H30B H 0.4444 0.2635 0.3647 0.095 Uiso 0.5 1 calc PR B 1
Cl33 Cl 0.34555(10) 0.2594(2) 0.33710(6) 0.0823(7) Uani 0.5 1 d PD C 2
Cl34 Cl 0.4158(6) 0.2935(11) 0.4004(3) 0.222(8) Uani 0.5 1 d PD C 2
C30' C 0.4067(4) 0.2220(9) 0.36721(18) 0.079(3) Uani 0.5 1 d PD C 2
H30C H 0.4004 0.1465 0.373 0.095 Uiso 0.5 1 calc PR C 2
H30D H 0.4459 0.2254 0.3581 0.095 Uiso 0.5 1 calc PR C 2
Cl41 Cl 0.6049(6) 0.4274(10) 0.5548(3) 0.055(2) Uani 0.5 1 d PD D 1
Cl42 Cl 0.55716(16) 0.3660(3) 0.48899(8) 0.0505(8) Uani 0.5 1 d PD D 1
C40 C 0.5837(7) 0.4703(12) 0.5150(3) 0.060(4) Uani 0.5 1 d PD D 1
H40A H 0.5506 0.525 0.5141 0.072 Uiso 0.5 1 calc PR D 1
H40B H 0.6201 0.5042 0.5077 0.072 Uiso 0.5 1 calc PR D 1
Cl43 Cl 0.4884(4) 0.3667(5) 0.47254(13) 0.114(2) Uani 0.5 1 d PD E 2
Cl44 Cl 0.4079(6) 0.5417(10) 0.4455(3) 0.065(3) Uani 0.5 1 d PD E 2
C40' C 0.4238(7) 0.4466(16) 0.4762(5) 0.113(11) Uani 0.5 1 d PD E 2
H40C H 0.3869 0.4001 0.4759 0.136 Uiso 0.5 1 calc PR E 2
H40D H 0.4313 0.4837 0.4973 0.136 Uiso 0.5 1 calc PR E 2



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C200 1.842(6) . ?
Ru1 C1 2.097(6) . ?
Ru1 Cl1 2.3694(12) . ?
Ru1 Cl2 2.3968(14) . ?
Ru1 P1 2.4409(17) . ?
Ru2 C400 1.826(6) . ?
Ru2 C6 2.100(6) . ?
Ru2 Cl3 2.3714(13) . ?
Ru2 Cl4 2.4014(13) . ?
Ru2 P2 2.4365(15) . ?
C1 N5 1.327(9) . ?
C1 N2 1.360(7) . ?
N2 C21 1.419(9) . ?
N2 C3 1.467(8) . ?
C21 C22 1.399(8) . ?
C21 C28A 1.444(9) . ?
C22 C23 1.400(10) . ?
C22 N241 1.420(9) . ?
C23 C24 1.366(10) . ?
C23 H23 0.95 . ?
C24 C24A 1.414(9) . ?
C24 H24 0.95 . ?
C24A C28A 1.416(9) . ?
C24A C25 1.428(10) . ?
C25 C26 1.363(10) . ?
C25 H25 0.95 . ?
C26 C27 1.414(11) . ?
C26 H26 0.95 . ?
C27 C28 1.364(10) . ?
C27 H27 0.95 . ?
C28 C28A 1.424(8) . ?
C28 H28 0.95 . ?
N241 C242 1.466(8) . ?
N241 C246 1.473(9) . ?
C242 C243 1.500(10) . ?
C242 H24A 0.99 . ?
C242 H24B 0.99 . ?
C243 O244 1.435(9) . ?
C243 H24C 0.99 . ?
C243 H24D 0.99 . ?
O244 C245 1.410(8) . ?
C245 C246 1.528(11) . ?
C245 H24E 0.99 . ?
C245 H24F 0.99 . ?
C246 H24G 0.99 . ?
C246 H24H 0.99 . ?
C3 C4 1.496(9) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.482(7) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.435(8) . ?
C51 C52 1.394(9) . ?
C51 C58A 1.409(8) . ?
C52 C53 1.413(10) . ?
C52 N541 1.430(8) . ?
C53 C54 1.355(9) . ?
C53 H53 0.95 . ?
C54 C54A 1.419(9) . ?
C54 H54 0.95 . ?
C54A C55 1.411(9) . ?
C54A C58A 1.431(9) . ?
C55 C56 1.366(9) . ?
C55 H55 0.95 . ?
C56 C57 1.411(9) . ?
C56 H56 0.95 . ?
C57 C58 1.368(9) . ?
C57 H57 0.95 . ?
C58 C58A 1.410(8) . ?
C58 H58 0.95 . ?
N541 C546 1.457(10) . ?
N541 C542 1.459(11) . ?
C542 C543 1.495(9) . ?
C542 H54A 0.99 . ?
C542 H54B 0.99 . ?
C543 O544 1.433(11) . ?
C543 H54C 0.99 . ?
C543 H54D 0.99 . ?
O544 C545 1.394(12) . ?
C545 C546 1.540(11) . ?
C545 H54E 0.99 . ?
C545 H54F 0.99 . ?
C546 H54G 0.99 . ?
C546 H54H 0.99 . ?
C200 C201 1.467(8) . ?
C200 H200 0.95 . ?
C201 C206 1.401(9) . ?
C201 C202 1.406(8) . ?
C202 C203 1.391(9) . ?
C202 H202 0.95 . ?
C203 C204 1.378(9) . ?
C203 H203 0.95 . ?
C204 C205 1.380(10) . ?
C204 H204 0.95 . ?
C205 C206 1.392(9) . ?
C205 H205 0.95 . ?
C206 H206 0.95 . ?
P1 C121 1.852(5) . ?
P1 C131 1.861(6) . ?
P1 C111 1.882(5) . ?
C111 C116 1.528(9) . ?
C111 C112 1.534(8) . ?
C111 H111 1 . ?
C112 C113 1.536(8) . ?
C112 H11A 0.99 . ?
C112 H11B 0.99 . ?
C113 C114 1.528(10) . ?
C113 H11C 0.99 . ?
C113 H11D 0.99 . ?
C114 C115 1.519(9) . ?
C114 H11E 0.99 . ?
C114 H11F 0.99 . ?
C115 C116 1.526(8) . ?
C115 H11G 0.99 . ?
C115 H11H 0.99 . ?
C116 H11I 0.99 . ?
C116 H11J 0.99 . ?
C121 C122 1.520(9) . ?
C121 C126 1.533(10) . ?
C121 H121 1 . ?
C122 C123 1.541(8) . ?
C122 H12A 0.99 . ?
C122 H12B 0.99 . ?
C123 C124 1.505(10) . ?
C123 H12C 0.99 . ?
C123 H12D 0.99 . ?
C124 C125 1.533(10) . ?
C124 H12E 0.99 . ?
C124 H12F 0.99 . ?
C125 C126 1.524(8) . ?
C125 H12G 0.99 . ?
C125 H12H 0.99 . ?
C126 H12I 0.99 . ?
C126 H12J 0.99 . ?
C131 C132 1.522(8) . ?
C131 C136 1.530(8) . ?
C131 H131 1 . ?
C132 C133 1.564(11) . ?
C132 H13A 0.99 . ?
C132 H13B 0.99 . ?
C133 C134 1.523(9) . ?
C133 H13C 0.99 . ?
C133 H13D 0.99 . ?
C134 C135 1.519(9) . ?
C134 H13E 0.99 . ?
C134 H13F 0.99 . ?
C135 C136 1.538(9) . ?
C135 H13G 0.99 . ?
C135 H13H 0.99 . ?
C136 H13I 0.99 . ?
C136 H13J 0.99 . ?
C6 N10 1.337(8) . ?
C6 N7 1.350(7) . ?
N7 C71 1.442(8) . ?
N7 C8 1.460(8) . ?
C71 C72 1.394(9) . ?
C71 C78A 1.431(9) . ?
C72 N741 1.392(8) . ?
C72 C73 1.441(10) . ?
C73 C74 1.336(10) . ?
C73 H73 0.95 . ?
C74 C74A 1.423(10) . ?
C74 H74 0.95 . ?
C74A C75 1.408(9) . ?
C74A C78A 1.409(9) . ?
C75 C76 1.351(11) . ?
C75 H75 0.95 . ?
C76 C77 1.402(11) . ?
C76 H76 0.95 . ?
C77 C78 1.354(9) . ?
C77 H77 0.95 . ?
C78 C78A 1.429(9) . ?
C78 H78 0.95 . ?
N741 C742 1.444(9) . ?
N741 C746 1.475(9) . ?
C742 C743 1.523(10) . ?
C742 H74A 0.99 . ?
C742 H74B 0.99 . ?
C743 O744 1.421(11) . ?
C743 H74C 0.99 . ?
C743 H74D 0.99 . ?
O744 C745 1.424(12) . ?
C745 C746 1.496(12) . ?
C745 H74E 0.99 . ?
C745 H74F 0.99 . ?
C746 H74G 0.99 . ?
C746 H74H 0.99 . ?
C8 C9 1.513(9) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 N10 1.468(7) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
N10 C101 1.427(7) . ?
C101 C102 1.407(8) . ?
C101 C18A 1.412(8) . ?
C102 N141 1.392(8) . ?
C102 C103 1.427(9) . ?
C103 C104 1.354(10) . ?
C103 H103 0.95 . ?
C104 C14A 1.396(9) . ?
C104 H104 0.95 . ?
C14A C18A 1.411(9) . ?
C14A C105 1.438(9) . ?
C105 C106 1.365(11) . ?
C105 H105 0.95 . ?
C106 C107 1.408(11) . ?
C106 H106 0.95 . ?
C107 C108 1.361(9) . ?
C107 H107 0.95 . ?
C108 C18A 1.421(9) . ?
C108 H108 0.95 . ?
N141 C142 1.451(9) . ?
N141 C146 1.455(8) . ?
C142 C143 1.517(10) . ?
C142 H14A 0.99 . ?
C142 H14B 0.99 . ?
C143 O144 1.434(9) . ?
C143 H14C 0.99 . ?
C143 H14D 0.99 . ?
O144 C145 1.430(10) . ?
C145 C146 1.492(10) . ?
C145 H14E 0.99 . ?
C145 H14F 0.99 . ?
C146 H14G 0.99 . ?
C146 H14H 0.99 . ?
C400 C401 1.456(9) . ?
C400 H400 0.95 . ?
C401 C402 1.394(11) . ?
C401 C406 1.417(11) . ?
C402 C403 1.385(11) . ?
C402 H402 0.95 . ?
C403 C404 1.372(17) . ?
C403 H403 0.95 . ?
C404 C405 1.354(17) . ?
C404 H404 0.95 . ?
C405 C406 1.406(14) . ?
C405 H405 0.95 . ?
C406 H406 0.95 . ?
P2 C221 1.861(6) . ?
P2 C211 1.873(5) . ?
P2 C231 1.873(6) . ?
C211 C216 1.535(9) . ?
C211 C212 1.549(8) . ?
C211 H211 1 . ?
C212 C213 1.528(8) . ?
C212 H21A 0.99 . ?
C212 H21B 0.99 . ?
C213 C214 1.520(10) . ?
C213 H21C 0.99 . ?
C213 H21D 0.99 . ?
C214 C215 1.524(10) . ?
C214 H21E 0.99 . ?
C214 H21F 0.99 . ?
C215 C216 1.522(8) . ?
C215 H21G 0.99 . ?
C215 H21H 0.99 . ?
C216 H21I 0.99 . ?
C216 H21J 0.99 . ?
C221 C226 1.526(9) . ?
C221 C222 1.528(9) . ?
C221 H221 1 . ?
C222 C223 1.532(8) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 C224 1.512(10) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
C224 C225 1.513(10) . ?
C224 H22E 0.99 . ?
C224 H22F 0.99 . ?
C225 C226 1.543(9) . ?
C225 H22G 0.99 . ?
C225 H22H 0.99 . ?
C226 H22I 0.99 . ?
C226 H22J 0.99 . ?
C231 C236 1.521(8) . ?
C231 C232 1.534(8) . ?
C231 H231 1 . ?
C232 C233 1.534(9) . ?
C232 H23A 0.99 . ?
C232 H23B 0.99 . ?
C233 C234 1.512(9) . ?
C233 H23C 0.99 . ?
C233 H23D 0.99 . ?
C234 C235 1.530(8) . ?
C234 H23E 0.99 . ?
C234 H23F 0.99 . ?
C235 C236 1.496(9) . ?
C235 H23G 0.99 . ?
C235 H23H 0.99 . ?
C236 H23I 0.99 . ?
C236 H23J 0.99 . ?
Cl11 C10 1.688(10) . ?
Cl12 C10 1.724(12) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
Cl13 C10' 1.623(15) . ?
Cl14 C10' 1.751(18) . ?
C10' H10C 0.99 . ?
C10' H10D 0.99 . ?
Cl21 C20 1.756(12) . ?
Cl22 C20 1.746(13) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
Cl23 C20' 1.75(2) . ?
Cl24 C20' 1.75(2) . ?
C20' H20C 0.99 . ?
C20' H20D 0.99 . ?
Cl31 C30 1.747(8) . ?
Cl32 C30 1.683(9) . ?
C30 H30A 0.99 . ?
C30 H30B 0.99 . ?
Cl41 C40 1.745(15) . ?
Cl42 C40 1.739(14) . ?
C40 H40A 0.99 . ?
C40 H40B 0.99 . ?
Cl43 C40' 1.753(17) . ?
Cl44 C40' 1.747(15) . ?
C40' H40C 0.99 . ?
C40' H40D 0.99 . ?

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
C200 Ru1 C1 95.2(3) . . ?
C200 Ru1 Cl1 105.89(18) . . ?
C1 Ru1 Cl1 94.34(14) . . ?
C200 Ru1 Cl2 88.95(19) . . ?
C1 Ru1 Cl2 86.50(15) . . ?
Cl1 Ru1 Cl2 164.97(6) . . ?
C200 Ru1 P1 97.32(19) . . ?
C1 Ru1 P1 165.39(18) . . ?
Cl1 Ru1 P1 89.49(5) . . ?
Cl2 Ru1 P1 86.20(6) . . ?
C400 Ru2 C6 97.6(2) . . ?
C400 Ru2 Cl3 105.8(2) . . ?
C6 Ru2 Cl3 89.03(14) . . ?
C400 Ru2 Cl4 88.9(2) . . ?
C6 Ru2 Cl4 92.00(13) . . ?
Cl3 Ru2 Cl4 165.06(6) . . ?
C400 Ru2 P2 95.46(19) . . ?
C6 Ru2 P2 166.76(17) . . ?
Cl3 Ru2 P2 89.72(5) . . ?
Cl4 Ru2 P2 85.88(5) . . ?
N5 C1 N2 107.5(5) . . ?
N5 C1 Ru1 129.6(4) . . ?
N2 C1 Ru1 121.9(5) . . ?
C1 N2 C21 126.5(5) . . ?
C1 N2 C3 111.0(5) . . ?
C21 N2 C3 122.4(5) . . ?
C22 C21 N2 121.0(6) . . ?
C22 C21 C28A 120.0(6) . . ?
N2 C21 C28A 118.8(5) . . ?
C21 C22 C23 119.0(6) . . ?
C21 C22 N241 119.6(6) . . ?
C23 C22 N241 121.3(5) . . ?
C24 C23 C22 122.3(6) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C24A 120.0(6) . . ?
C23 C24 H24 120 . . ?
C24A C24 H24 120 . . ?
C24 C24A C28A 119.8(6) . . ?
C24 C24A C25 121.2(6) . . ?
C28A C24A C25 119.0(6) . . ?
C26 C25 C24A 121.0(7) . . ?
C26 C25 H25 119.5 . . ?
C24A C25 H25 119.5 . . ?
C25 C26 C27 119.2(7) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C28 C27 C26 122.0(6) . . ?
C28 C27 H27 119 . . ?
C26 C27 H27 119 . . ?
C27 C28 C28A 119.6(6) . . ?
C27 C28 H28 120.2 . . ?
C28A C28 H28 120.2 . . ?
C24A C28A C28 119.2(6) . . ?
C24A C28A C21 118.6(5) . . ?
C28 C28A C21 122.2(6) . . ?
C22 N241 C242 115.7(6) . . ?
C22 N241 C246 113.6(5) . . ?
C242 N241 C246 109.1(5) . . ?
N241 C242 C243 108.0(6) . . ?
N241 C242 H24A 110.1 . . ?
C243 C242 H24A 110.1 . . ?
N241 C242 H24B 110.1 . . ?
C243 C242 H24B 110.1 . . ?
H24A C242 H24B 108.4 . . ?
O244 C243 C242 111.9(5) . . ?
O244 C243 H24C 109.2 . . ?
C242 C243 H24C 109.2 . . ?
O244 C243 H24D 109.2 . . ?
C242 C243 H24D 109.2 . . ?
H24C C243 H24D 107.9 . . ?
C245 O244 C243 109.5(5) . . ?
O244 C245 C246 112.0(7) . . ?
O244 C245 H24E 109.2 . . ?
C246 C245 H24E 109.2 . . ?
O244 C245 H24F 109.2 . . ?
C246 C245 H24F 109.2 . . ?
H24E C245 H24F 107.9 . . ?
N241 C246 C245 110.1(5) . . ?
N241 C246 H24G 109.6 . . ?
C245 C246 H24G 109.6 . . ?
N241 C246 H24H 109.6 . . ?
C245 C246 H24H 109.6 . . ?
H24G C246 H24H 108.1 . . ?
N2 C3 C4 102.0(5) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.2 . . ?
N5 C4 C3 101.1(5) . . ?
N5 C4 H4A 111.6 . . ?
C3 C4 H4A 111.6 . . ?
N5 C4 H4B 111.6 . . ?
C3 C4 H4B 111.6 . . ?
H4A C4 H4B 109.4 . . ?
C1 N5 C51 128.4(5) . . ?
C1 N5 C4 112.3(5) . . ?
C51 N5 C4 117.3(5) . . ?
C52 C51 C58A 121.3(6) . . ?
C52 C51 N5 118.7(5) . . ?
C58A C51 N5 118.9(5) . . ?
C51 C52 C53 118.1(6) . . ?
C51 C52 N541 120.6(6) . . ?
C53 C52 N541 121.3(6) . . ?
C54 C53 C52 121.5(6) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C53 C54 C54A 121.4(6) . . ?
C53 C54 H54 119.3 . . ?
C54A C54 H54 119.3 . . ?
C55 C54A C54 122.0(6) . . ?
C55 C54A C58A 120.0(5) . . ?
C54 C54A C58A 118.0(6) . . ?
C56 C55 C54A 120.8(6) . . ?
C56 C55 H55 119.6 . . ?
C54A C55 H55 119.6 . . ?
C55 C56 C57 119.0(6) . . ?
C55 C56 H56 120.5 . . ?
C57 C56 H56 120.5 . . ?
C58 C57 C56 121.7(6) . . ?
C58 C57 H57 119.2 . . ?
C56 C57 H57 119.2 . . ?
C57 C58 C58A 120.7(6) . . ?
C57 C58 H58 119.7 . . ?
C58A C58 H58 119.7 . . ?
C51 C58A C58 123.3(6) . . ?
C51 C58A C54A 119.0(5) . . ?
C58 C58A C54A 117.7(5) . . ?
C52 N541 C546 116.2(6) . . ?
C52 N541 C542 116.1(6) . . ?
C546 N541 C542 110.5(6) . . ?
N541 C542 C543 110.2(7) . . ?
N541 C542 H54A 109.6 . . ?
C543 C542 H54A 109.6 . . ?
N541 C542 H54B 109.6 . . ?
C543 C542 H54B 109.6 . . ?
H54A C542 H54B 108.1 . . ?
O544 C543 C542 111.7(8) . . ?
O544 C543 H54C 109.3 . . ?
C542 C543 H54C 109.3 . . ?
O544 C543 H54D 109.3 . . ?
C542 C543 H54D 109.3 . . ?
H54C C543 H54D 107.9 . . ?
C545 O544 C543 109.0(6) . . ?
O544 C545 C546 111.7(7) . . ?
O544 C545 H54E 109.3 . . ?
C546 C545 H54E 109.3 . . ?
O544 C545 H54F 109.3 . . ?
C546 C545 H54F 109.3 . . ?
H54E C545 H54F 107.9 . . ?
N541 C546 C545 107.2(7) . . ?
N541 C546 H54G 110.3 . . ?
C545 C546 H54G 110.3 . . ?
N541 C546 H54H 110.3 . . ?
C545 C546 H54H 110.3 . . ?
H54G C546 H54H 108.5 . . ?
C201 C200 Ru1 136.1(4) . . ?
C201 C200 H200 111.9 . . ?
Ru1 C200 H200 111.9 . . ?
C206 C201 C202 118.3(6) . . ?
C206 C201 C200 116.8(5) . . ?
C202 C201 C200 124.9(5) . . ?
C203 C202 C201 119.7(6) . . ?
C203 C202 H202 120.1 . . ?
C201 C202 H202 120.1 . . ?
C204 C203 C202 121.2(6) . . ?
C204 C203 H203 119.4 . . ?
C202 C203 H203 119.4 . . ?
C203 C204 C205 119.7(6) . . ?
C203 C204 H204 120.1 . . ?
C205 C204 H204 120.1 . . ?
C204 C205 C206 120.0(6) . . ?
C204 C205 H205 120 . . ?
C206 C205 H205 120 . . ?
C205 C206 C201 120.9(6) . . ?
C205 C206 H206 119.5 . . ?
C201 C206 H206 119.5 . . ?
C121 P1 C131 102.6(3) . . ?
C121 P1 C111 109.4(3) . . ?
C131 P1 C111 101.8(3) . . ?
C121 P1 Ru1 114.7(2) . . ?
C131 P1 Ru1 111.8(2) . . ?
C111 P1 Ru1 115.1(2) . . ?
C116 C111 C112 110.0(5) . . ?
C116 C111 P1 118.0(4) . . ?
C112 C111 P1 111.8(4) . . ?
C116 C111 H111 105.3 . . ?
C112 C111 H111 105.3 . . ?
P1 C111 H111 105.3 . . ?
C111 C112 C113 110.4(5) . . ?
C111 C112 H11A 109.6 . . ?
C113 C112 H11A 109.6 . . ?
C111 C112 H11B 109.6 . . ?
C113 C112 H11B 109.6 . . ?
H11A C112 H11B 108.1 . . ?
C114 C113 C112 110.0(5) . . ?
C114 C113 H11C 109.7 . . ?
C112 C113 H11C 109.7 . . ?
C114 C113 H11D 109.7 . . ?
C112 C113 H11D 109.7 . . ?
H11C C113 H11D 108.2 . . ?
C115 C114 C113 111.2(5) . . ?
C115 C114 H11E 109.4 . . ?
C113 C114 H11E 109.4 . . ?
C115 C114 H11F 109.4 . . ?
C113 C114 H11F 109.4 . . ?
H11E C114 H11F 108 . . ?
C114 C115 C116 112.7(5) . . ?
C114 C115 H11G 109 . . ?
C116 C115 H11G 109 . . ?
C114 C115 H11H 109 . . ?
C116 C115 H11H 109 . . ?
H11G C115 H11H 107.8 . . ?
C115 C116 C111 110.1(5) . . ?
C115 C116 H11I 109.6 . . ?
C111 C116 H11I 109.6 . . ?
C115 C116 H11J 109.6 . . ?
C111 C116 H11J 109.6 . . ?
H11I C116 H11J 108.1 . . ?
C122 C121 C126 111.8(5) . . ?
C122 C121 P1 115.4(5) . . ?
C126 C121 P1 113.9(4) . . ?
C122 C121 H121 104.8 . . ?
C126 C121 H121 104.8 . . ?
P1 C121 H121 104.8 . . ?
C121 C122 C123 109.7(6) . . ?
C121 C122 H12A 109.7 . . ?
C123 C122 H12A 109.7 . . ?
C121 C122 H12B 109.7 . . ?
C123 C122 H12B 109.7 . . ?
H12A C122 H12B 108.2 . . ?
C124 C123 C122 112.7(5) . . ?
C124 C123 H12C 109.1 . . ?
C122 C123 H12C 109.1 . . ?
C124 C123 H12D 109.1 . . ?
C122 C123 H12D 109.1 . . ?
H12C C123 H12D 107.8 . . ?
C123 C124 C125 109.9(5) . . ?
C123 C124 H12E 109.7 . . ?
C125 C124 H12E 109.7 . . ?
C123 C124 H12F 109.7 . . ?
C125 C124 H12F 109.7 . . ?
H12E C124 H12F 108.2 . . ?
C126 C125 C124 111.5(6) . . ?
C126 C125 H12G 109.3 . . ?
C124 C125 H12G 109.3 . . ?
C126 C125 H12H 109.3 . . ?
C124 C125 H12H 109.3 . . ?
H12G C125 H12H 108 . . ?
C125 C126 C121 112.9(5) . . ?
C125 C126 H12I 109 . . ?
C121 C126 H12I 109 . . ?
C125 C126 H12J 109 . . ?
C121 C126 H12J 109 . . ?
H12I C126 H12J 107.8 . . ?
C132 C131 C136 108.7(5) . . ?
C132 C131 P1 116.5(5) . . ?
C136 C131 P1 112.1(4) . . ?
C132 C131 H131 106.3 . . ?
C136 C131 H131 106.3 . . ?
P1 C131 H131 106.3 . . ?
C131 C132 C133 109.4(6) . . ?
C131 C132 H13A 109.8 . . ?
C133 C132 H13A 109.8 . . ?
C131 C132 H13B 109.8 . . ?
C133 C132 H13B 109.8 . . ?
H13A C132 H13B 108.2 . . ?
C134 C133 C132 110.4(6) . . ?
C134 C133 H13C 109.6 . . ?
C132 C133 H13C 109.6 . . ?
C134 C133 H13D 109.6 . . ?
C132 C133 H13D 109.6 . . ?
H13C C133 H13D 108.1 . . ?
C135 C134 C133 112.0(5) . . ?
C135 C134 H13E 109.2 . . ?
C133 C134 H13E 109.2 . . ?
C135 C134 H13F 109.2 . . ?
C133 C134 H13F 109.2 . . ?
H13E C134 H13F 107.9 . . ?
C134 C135 C136 110.6(6) . . ?
C134 C135 H13G 109.5 . . ?
C136 C135 H13G 109.5 . . ?
C134 C135 H13H 109.5 . . ?
C136 C135 H13H 109.5 . . ?
H13G C135 H13H 108.1 . . ?
C131 C136 C135 109.9(5) . . ?
C131 C136 H13I 109.7 . . ?
C135 C136 H13I 109.7 . . ?
C131 C136 H13J 109.7 . . ?
C135 C136 H13J 109.7 . . ?
H13I C136 H13J 108.2 . . ?
N10 C6 N7 107.7(5) . . ?
N10 C6 Ru2 129.5(4) . . ?
N7 C6 Ru2 122.6(4) . . ?
C6 N7 C71 127.5(5) . . ?
C6 N7 C8 112.1(5) . . ?
C71 N7 C8 119.0(5) . . ?
C72 C71 C78A 120.7(6) . . ?
C72 C71 N7 122.2(6) . . ?
C78A C71 N7 116.8(5) . . ?
N741 C72 C71 128.1(6) . . ?
N741 C72 C73 115.2(5) . . ?
C71 C72 C73 116.4(6) . . ?
C74 C73 C72 123.2(6) . . ?
C74 C73 H73 118.4 . . ?
C72 C73 H73 118.4 . . ?
C73 C74 C74A 121.6(6) . . ?
C73 C74 H74 119.2 . . ?
C74A C74 H74 119.2 . . ?
C75 C74A C78A 120.3(6) . . ?
C75 C74A C74 122.8(7) . . ?
C78A C74A C74 116.9(6) . . ?
C76 C75 C74A 121.4(7) . . ?
C76 C75 H75 119.3 . . ?
C74A C75 H75 119.3 . . ?
C75 C76 C77 119.1(6) . . ?
C75 C76 H76 120.5 . . ?
C77 C76 H76 120.5 . . ?
C78 C77 C76 121.2(7) . . ?
C78 C77 H77 119.4 . . ?
C76 C77 H77 119.4 . . ?
C77 C78 C78A 121.4(7) . . ?
C77 C78 H78 119.3 . . ?
C78A C78 H78 119.3 . . ?
C74A C78A C78 116.6(6) . . ?
C74A C78A C71 121.2(6) . . ?
C78 C78A C71 122.1(6) . . ?
C72 N741 C742 123.2(5) . . ?
C72 N741 C746 120.6(6) . . ?
C742 N741 C746 110.1(5) . . ?
N741 C742 C743 112.5(6) . . ?
N741 C742 H74A 109.1 . . ?
C743 C742 H74A 109.1 . . ?
N741 C742 H74B 109.1 . . ?
C743 C742 H74B 109.1 . . ?
H74A C742 H74B 107.8 . . ?
O744 C743 C742 110.6(8) . . ?
O744 C743 H74C 109.5 . . ?
C742 C743 H74C 109.5 . . ?
O744 C743 H74D 109.5 . . ?
C742 C743 H74D 109.5 . . ?
H74C C743 H74D 108.1 . . ?
C743 O744 C745 108.8(7) . . ?
O744 C745 C746 110.4(7) . . ?
O744 C745 H74E 109.6 . . ?
C746 C745 H74E 109.6 . . ?
O744 C745 H74F 109.6 . . ?
C746 C745 H74F 109.6 . . ?
H74E C745 H74F 108.1 . . ?
N741 C746 C745 111.7(7) . . ?
N741 C746 H74G 109.3 . . ?
C745 C746 H74G 109.3 . . ?
N741 C746 H74H 109.3 . . ?
C745 C746 H74H 109.3 . . ?
H74G C746 H74H 107.9 . . ?
N7 C8 C9 101.7(4) . . ?
N7 C8 H8A 111.4 . . ?
C9 C8 H8A 111.4 . . ?
N7 C8 H8B 111.4 . . ?
C9 C8 H8B 111.4 . . ?
H8A C8 H8B 109.3 . . ?
N10 C9 C8 102.2(5) . . ?
N10 C9 H9A 111.3 . . ?
C8 C9 H9A 111.3 . . ?
N10 C9 H9B 111.3 . . ?
C8 C9 H9B 111.3 . . ?
H9A C9 H9B 109.2 . . ?
C6 N10 C101 128.6(5) . . ?
C6 N10 C9 112.2(5) . . ?
C101 N10 C9 117.6(5) . . ?
C102 C101 C18A 120.5(5) . . ?
C102 C101 N10 118.8(5) . . ?
C18A C101 N10 119.8(5) . . ?
N141 C102 C101 121.9(5) . . ?
N141 C102 C103 120.7(5) . . ?
C101 C102 C103 117.1(6) . . ?
C104 C103 C102 121.5(6) . . ?
C104 C103 H103 119.2 . . ?
C102 C103 H103 119.2 . . ?
C103 C104 C14A 122.0(6) . . ?
C103 C104 H104 119 . . ?
C14A C104 H104 119 . . ?
C104 C14A C18A 118.1(6) . . ?
C104 C14A C105 121.5(6) . . ?
C18A C14A C105 120.4(6) . . ?
C106 C105 C14A 120.1(7) . . ?
C106 C105 H105 120 . . ?
C14A C105 H105 120 . . ?
C105 C106 C107 119.4(6) . . ?
C105 C106 H106 120.3 . . ?
C107 C106 H106 120.3 . . ?
C108 C107 C106 121.4(7) . . ?
C108 C107 H107 119.3 . . ?
C106 C107 H107 119.3 . . ?
C107 C108 C18A 121.5(6) . . ?
C107 C108 H108 119.2 . . ?
C18A C108 H108 119.2 . . ?
C14A C18A C101 120.3(6) . . ?
C14A C18A C108 117.1(6) . . ?
C101 C18A C108 122.5(6) . . ?
C102 N141 C142 118.9(5) . . ?
C102 N141 C146 118.3(6) . . ?
C142 N141 C146 109.8(5) . . ?
N141 C142 C143 110.2(6) . . ?
N141 C142 H14A 109.6 . . ?
C143 C142 H14A 109.6 . . ?
N141 C142 H14B 109.6 . . ?
C143 C142 H14B 109.6 . . ?
H14A C142 H14B 108.1 . . ?
O144 C143 C142 110.4(6) . . ?
O144 C143 H14C 109.6 . . ?
C142 C143 H14C 109.6 . . ?
O144 C143 H14D 109.6 . . ?
C142 C143 H14D 109.6 . . ?
H14C C143 H14D 108.1 . . ?
C145 O144 C143 109.7(5) . . ?
O144 C145 C146 112.3(6) . . ?
O144 C145 H14E 109.1 . . ?
C146 C145 H14E 109.1 . . ?
O144 C145 H14F 109.1 . . ?
C146 C145 H14F 109.1 . . ?
H14E C145 H14F 107.9 . . ?
N141 C146 C145 109.5(6) . . ?
N141 C146 H14G 109.8 . . ?
C145 C146 H14G 109.8 . . ?
N141 C146 H14H 109.8 . . ?
C145 C146 H14H 109.8 . . ?
H14G C146 H14H 108.2 . . ?
C401 C400 Ru2 136.2(5) . . ?
C401 C400 H400 111.9 . . ?
Ru2 C400 H400 111.9 . . ?
C402 C401 C406 116.9(7) . . ?
C402 C401 C400 125.1(7) . . ?
C406 C401 C400 118.1(7) . . ?
C403 C402 C401 122.0(10) . . ?
C403 C402 H402 119 . . ?
C401 C402 H402 119 . . ?
C404 C403 C402 119.7(12) . . ?
C404 C403 H403 120.1 . . ?
C402 C403 H403 120.1 . . ?
C405 C404 C403 120.8(10) . . ?
C405 C404 H404 119.6 . . ?
C403 C404 H404 119.6 . . ?
C404 C405 C406 120.4(10) . . ?
C404 C405 H405 119.8 . . ?
C406 C405 H405 119.8 . . ?
C405 C406 C401 120.1(10) . . ?
C405 C406 H406 119.9 . . ?
C401 C406 H406 119.9 . . ?
C221 P2 C211 109.7(3) . . ?
C221 P2 C231 103.5(3) . . ?
C211 P2 C231 101.9(3) . . ?
C221 P2 Ru2 115.6(2) . . ?
C211 P2 Ru2 114.1(2) . . ?
C231 P2 Ru2 110.66(19) . . ?
C216 C211 C212 109.5(5) . . ?
C216 C211 P2 118.8(4) . . ?
C212 C211 P2 111.8(4) . . ?
C216 C211 H211 105.2 . . ?
C212 C211 H211 105.2 . . ?
P2 C211 H211 105.2 . . ?
C213 C212 C211 109.7(5) . . ?
C213 C212 H21A 109.7 . . ?
C211 C212 H21A 109.7 . . ?
C213 C212 H21B 109.7 . . ?
C211 C212 H21B 109.7 . . ?
H21A C212 H21B 108.2 . . ?
C214 C213 C212 110.9(5) . . ?
C214 C213 H21C 109.5 . . ?
C212 C213 H21C 109.5 . . ?
C214 C213 H21D 109.5 . . ?
C212 C213 H21D 109.5 . . ?
H21C C213 H21D 108.1 . . ?
C213 C214 C215 111.3(5) . . ?
C213 C214 H21E 109.4 . . ?
C215 C214 H21E 109.4 . . ?
C213 C214 H21F 109.4 . . ?
C215 C214 H21F 109.4 . . ?
H21E C214 H21F 108 . . ?
C216 C215 C214 111.8(6) . . ?
C216 C215 H21G 109.2 . . ?
C214 C215 H21G 109.2 . . ?
C216 C215 H21H 109.2 . . ?
C214 C215 H21H 109.2 . . ?
H21G C215 H21H 107.9 . . ?
C215 C216 C211 109.3(5) . . ?
C215 C216 H21I 109.8 . . ?
C211 C216 H21I 109.8 . . ?
C215 C216 H21J 109.8 . . ?
C211 C216 H21J 109.8 . . ?
H21I C216 H21J 108.3 . . ?
C226 C221 C222 112.2(5) . . ?
C226 C221 P2 114.6(4) . . ?
C222 C221 P2 114.7(4) . . ?
C226 C221 H221 104.6 . . ?
C222 C221 H221 104.6 . . ?
P2 C221 H221 104.6 . . ?
C221 C222 C223 111.1(5) . . ?
C221 C222 H22A 109.4 . . ?
C223 C222 H22A 109.4 . . ?
C221 C222 H22B 109.4 . . ?
C223 C222 H22B 109.4 . . ?
H22A C222 H22B 108 . . ?
C224 C223 C222 111.6(5) . . ?
C224 C223 H22C 109.3 . . ?
C222 C223 H22C 109.3 . . ?
C224 C223 H22D 109.3 . . ?
C222 C223 H22D 109.3 . . ?
H22C C223 H22D 108 . . ?
C223 C224 C225 111.6(6) . . ?
C223 C224 H22E 109.3 . . ?
C225 C224 H22E 109.3 . . ?
C223 C224 H22F 109.3 . . ?
C225 C224 H22F 109.3 . . ?
H22E C224 H22F 108 . . ?
C224 C225 C226 111.7(6) . . ?
C224 C225 H22G 109.3 . . ?
C226 C225 H22G 109.3 . . ?
C224 C225 H22H 109.3 . . ?
C226 C225 H22H 109.3 . . ?
H22G C225 H22H 107.9 . . ?
C221 C226 C225 110.9(5) . . ?
C221 C226 H22I 109.5 . . ?
C225 C226 H22I 109.5 . . ?
C221 C226 H22J 109.5 . . ?
C225 C226 H22J 109.5 . . ?
H22I C226 H22J 108.1 . . ?
C236 C231 C232 109.1(5) . . ?
C236 C231 P2 111.7(4) . . ?
C232 C231 P2 114.5(4) . . ?
C236 C231 H231 107 . . ?
C232 C231 H231 107 . . ?
P2 C231 H231 107 . . ?
C231 C232 C233 109.7(5) . . ?
C231 C232 H23A 109.7 . . ?
C233 C232 H23A 109.7 . . ?
C231 C232 H23B 109.7 . . ?
C233 C232 H23B 109.7 . . ?
H23A C232 H23B 108.2 . . ?
C234 C233 C232 112.0(5) . . ?
C234 C233 H23C 109.2 . . ?
C232 C233 H23C 109.2 . . ?
C234 C233 H23D 109.2 . . ?
C232 C233 H23D 109.2 . . ?
H23C C233 H23D 107.9 . . ?
C233 C234 C235 111.4(5) . . ?
C233 C234 H23E 109.3 . . ?
C235 C234 H23E 109.3 . . ?
C233 C234 H23F 109.3 . . ?
C235 C234 H23F 109.3 . . ?
H23E C234 H23F 108 . . ?
C236 C235 C234 112.4(5) . . ?
C236 C235 H23G 109.1 . . ?
C234 C235 H23G 109.1 . . ?
C236 C235 H23H 109.1 . . ?
C234 C235 H23H 109.1 . . ?
H23G C235 H23H 107.9 . . ?
C235 C236 C231 110.5(5) . . ?
C235 C236 H23I 109.6 . . ?
C231 C236 H23I 109.6 . . ?
C235 C236 H23J 109.6 . . ?
C231 C236 H23J 109.6 . . ?
H23I C236 H23J 108.1 . . ?
Cl11 C10 Cl12 115.7(7) . . ?
Cl11 C10 H10A 108.4 . . ?
Cl12 C10 H10A 108.4 . . ?
Cl11 C10 H10B 108.4 . . ?
Cl12 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
Cl13 C10' Cl14 113.3(12) . . ?
Cl13 C10' H10C 108.9 . . ?
Cl14 C10' H10C 108.9 . . ?
Cl13 C10' H10D 108.9 . . ?
Cl14 C10' H10D 108.9 . . ?
H10C C10' H10D 107.7 . . ?
Cl22 C20 Cl21 111.4(8) . . ?
Cl22 C20 H20A 109.3 . . ?
Cl21 C20 H20A 109.3 . . ?
Cl22 C20 H20B 109.3 . . ?
Cl21 C20 H20B 109.3 . . ?
H20A C20 H20B 108 . . ?
Cl24 C20' Cl23 111.0(16) . . ?
Cl24 C20' H20C 109.4 . . ?
Cl23 C20' H20C 109.4 . . ?
Cl24 C20' H20D 109.4 . . ?
Cl23 C20' H20D 109.4 . . ?
H20C C20' H20D 108 . . ?
Cl32 C30 Cl31 111.4(5) . . ?
Cl32 C30 H30A 109.3 . . ?
Cl31 C30 H30A 109.4 . . ?
Cl32 C30 H30B 109.4 . . ?
Cl31 C30 H30B 109.4 . . ?
H30A C30 H30B 108 . . ?
Cl42 C40 Cl41 112.4(9) . . ?
Cl42 C40 H40A 109.1 . . ?
Cl41 C40 H40A 109.1 . . ?
Cl42 C40 H40B 109.1 . . ?
Cl41 C40 H40B 109.1 . . ?
H40A C40 H40B 107.9 . . ?
Cl44 C40' Cl43 112.9(10) . . ?
Cl44 C40' H40C 109 . . ?
Cl43 C40' H40C 109 . . ?
Cl44 C40' H40D 109 . . ?
Cl43 C40' H40D 109 . . ?
H40C C40' H40D 107.8 . . ?

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

data_rda538
_database_code_depnum_ccdc_archive 'CCDC 1518963'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

_audit_creation_date             2015-12-16T12:49:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C60 H79 Cl6 N4 P Ru'
_chemical_formula_moiety         'C58 H75 Cl2 N4 P Ru, 2(C H2 Cl2)'
_chemical_formula_weight         1201.01

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

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

_cell_length_a                   12.5108(3)
_cell_length_b                   14.5880(4)
_cell_length_c                   15.8611(4)
_cell_angle_alpha                81.376(2)
_cell_angle_beta                 82.250(2)
_cell_angle_gamma                86.811(2)
_cell_volume                     2834.05(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15471
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      67.152

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

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.067
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             1256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 1 0.0302
0 -2 -1 0.0516
-1 -1 -1 0.0266
2 1 1 0.0239
0 -2 1 0.0535
-2 -1 4 0.0702
1 0 -2 0.0468
-1 0 -1 0.0258


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

_exptl_absorpt_coefficient_mu    5.431
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
       CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)

;
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.818

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

_diffrn_source                   'sealed X-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      -0.0099627
_diffrn_orient_matrix_ub_12      -0.0779333
_diffrn_orient_matrix_ub_13      0.0774682
_diffrn_orient_matrix_ub_21      0.0721355
_diffrn_orient_matrix_ub_22      -0.06481
_diffrn_orient_matrix_ub_23      -0.0537096
_diffrn_orient_matrix_ub_31      0.100804
_diffrn_orient_matrix_ub_32      0.0339108
_diffrn_orient_matrix_ub_33      0.0304313
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_number            25358
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.841
_diffrn_reflns_theta_max         67.382
_diffrn_reflns_theta_full        67.382
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_reflns_number_total             10065
_reflns_number_gt                8851
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


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

_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 One phosphine cyclohexyl ring, the benzylidene group and one solvent
dichloromethane molecule were all found to be disordered and were refined
with site occupancies constrained to 0.5 from considerations of intermolecular
interactions. Geometries of the disordered groups were restrained to ideal values.

;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²+6.0524P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10065
_refine_ls_number_parameters     771
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.169
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.095

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.28594(2) 0.75713(2) 0.26174(2) 0.02105(10) Uani 1 d . .
Cl1 Cl 0.41611(7) 0.81963(7) 0.33240(7) 0.0380(2) Uani 1 d . .
Cl2 Cl 0.13944(7) 0.72723(7) 0.18934(6) 0.0319(2) Uani 1 d . .
C1 C 0.3917(3) 0.7828(2) 0.1480(2) 0.0218(7) Uani 1 d . .
N2 N 0.4743(2) 0.7286(2) 0.11566(18) 0.0228(6) Uani 1 d . .
C21 C 0.4945(3) 0.6316(3) 0.1367(2) 0.0265(8) Uani 1 d . .
C22 C 0.5935(3) 0.6004(3) 0.1629(2) 0.0310(8) Uani 1 d . .
N221 N 0.6727(3) 0.6630(3) 0.1682(2) 0.0367(8) Uani 1 d . .
C222 C 0.7860(3) 0.6291(4) 0.1598(3) 0.0490(12) Uani 1 d . .
H22A H 0.7973 0.5835 0.1188 0.059 Uiso 1 calc . .
H22B H 0.8042 0.5981 0.2162 0.059 Uiso 1 calc . .
C223 C 0.8577(4) 0.7105(4) 0.1277(3) 0.0595(15) Uani 1 d . .
H22C H 0.9341 0.6883 0.1247 0.071 Uiso 1 calc . .
H22D H 0.8439 0.7369 0.0688 0.071 Uiso 1 calc . .
C224 C 0.8394(4) 0.7856(5) 0.1844(3) 0.0626(16) Uani 1 d . .
H22E H 0.8802 0.8407 0.1565 0.075 Uiso 1 calc . .
H22F H 0.8664 0.7633 0.24 0.075 Uiso 1 calc . .
C225 C 0.7183(4) 0.8129(4) 0.2004(4) 0.0538(13) Uani 1 d . .
H22G H 0.7065 0.8551 0.2444 0.065 Uiso 1 calc . .
H22H H 0.6948 0.8465 0.1466 0.065 Uiso 1 calc . .
C226 C 0.6514(3) 0.7282(3) 0.2303(3) 0.0414(10) Uani 1 d . .
H22I H 0.6695 0.698 0.2871 0.05 Uiso 1 calc . .
H22J H 0.5738 0.747 0.2368 0.05 Uiso 1 calc . .
C23 C 0.6150(4) 0.5029(3) 0.1770(3) 0.0420(11) Uani 1 d . .
H23 H 0.6792 0.4798 0.2 0.05 Uiso 1 calc . .
C24A C 0.4516(4) 0.4733(3) 0.1231(3) 0.0378(10) Uani 1 d . .
C25 C 0.3846(4) 0.4123(3) 0.0949(3) 0.0476(12) Uani 1 d . .
H25 H 0.4007 0.3475 0.1043 0.057 Uiso 1 calc . .
C26 C 0.2985(5) 0.4440(3) 0.0550(3) 0.0524(13) Uani 1 d . .
H26 H 0.2557 0.4017 0.0355 0.063 Uiso 1 calc . .
C27 C 0.2722(4) 0.5395(3) 0.0424(3) 0.0430(10) Uani 1 d . .
H27 H 0.212 0.5618 0.0135 0.052 Uiso 1 calc . .
C28 C 0.3326(3) 0.6007(3) 0.0714(2) 0.0311(8) Uani 1 d . .
H28 H 0.3122 0.6649 0.0644 0.037 Uiso 1 calc . .
C28A C 0.4249(3) 0.5701(3) 0.1117(2) 0.0282(8) Uani 1 d . .
C2 C 0.5469(4) 0.4425(3) 0.1586(3) 0.0445(11) Uani 1 d . .
H2 H 0.5634 0.3779 0.1698 0.053 Uiso 1 calc . .
C3 C 0.5301(3) 0.7735(3) 0.0330(2) 0.0276(8) Uani 1 d . .
H3A H 0.5043 0.7511 -0.0164 0.033 Uiso 1 calc . .
H3B H 0.6093 0.7628 0.0297 0.033 Uiso 1 calc . .
C4 C 0.4985(3) 0.8743(3) 0.0360(2) 0.0304(8) Uani 1 d . .
H4A H 0.5542 0.9068 0.0577 0.037 Uiso 1 calc . .
H4B H 0.4846 0.9068 -0.0211 0.037 Uiso 1 calc . .
N5 N 0.3985(2) 0.8657(2) 0.09736(19) 0.0240(6) Uani 1 d . .
C51 C 0.3269(3) 0.9452(3) 0.1010(2) 0.0272(8) Uani 1 d . .
C52 C 0.2416(3) 0.9559(3) 0.0530(2) 0.0347(9) Uani 1 d . .
N521 N 0.2216(3) 0.8867(3) 0.0031(2) 0.0367(8) Uani 1 d . .
C522 C 0.2775(4) 0.8991(4) -0.0850(3) 0.0580(14) Uani 1 d . .
H52A H 0.3532 0.9154 -0.0845 0.07 Uiso 1 calc . .
H52B H 0.2419 0.9507 -0.1202 0.07 Uiso 1 calc . .
C523 C 0.2756(4) 0.8100(5) -0.1246(3) 0.0627(16) Uani 1 d . .
H52C H 0.3134 0.8189 -0.184 0.075 Uiso 1 calc . .
H52D H 0.3135 0.7588 -0.0907 0.075 Uiso 1 calc . .
C524 C 0.1591(5) 0.7847(5) -0.1255(3) 0.0668(17) Uani 1 d . .
H52E H 0.1576 0.7237 -0.1454 0.08 Uiso 1 calc . .
H52F H 0.1239 0.8317 -0.1656 0.08 Uiso 1 calc . .
C525 C 0.0980(4) 0.7809(4) -0.0346(3) 0.0524(13) Uani 1 d . .
H52G H 0.0208 0.7707 -0.0364 0.063 Uiso 1 calc . .
H52H H 0.1269 0.7276 0.0031 0.063 Uiso 1 calc . .
C526 C 0.1077(3) 0.8684(4) 0.0030(3) 0.0476(12) Uani 1 d . .
H52I H 0.0728 0.9212 -0.0313 0.057 Uiso 1 calc . .
H52J H 0.0702 0.8618 0.0626 0.057 Uiso 1 calc . .
C53 C 0.1786(4) 1.0407(4) 0.0514(3) 0.0492(12) Uani 1 d . .
H53 H 0.1185 1.049 0.0199 0.059 Uiso 1 calc . .
C54 C 0.2024(4) 1.1095(3) 0.0937(3) 0.0522(13) Uani 1 d . .
H54 H 0.1579 1.1645 0.0921 0.063 Uiso 1 calc . .
C54A C 0.2912(4) 1.1012(3) 0.1400(3) 0.0425(11) Uani 1 d . .
C55 C 0.3201(5) 1.1738(3) 0.1827(3) 0.0556(14) Uani 1 d . .
H55 H 0.277 1.2296 0.1813 0.067 Uiso 1 calc . .
C56 C 0.4083(5) 1.1646(3) 0.2257(3) 0.0610(16) Uani 1 d . .
H56 H 0.4273 1.2142 0.2526 0.073 Uiso 1 calc . .
C57 C 0.4705(4) 1.0821(3) 0.2299(3) 0.0465(11) Uani 1 d . .
H57 H 0.5315 1.0758 0.2604 0.056 Uiso 1 calc . .
C58 C 0.4450(3) 1.0098(3) 0.1909(3) 0.0342(9) Uani 1 d . .
H58 H 0.4884 0.9541 0.1948 0.041 Uiso 1 calc . .
C58A C 0.3550(3) 1.0173(3) 0.1449(3) 0.0321(8) Uani 1 d . .
P1 P 0.15511(7) 0.77851(6) 0.38637(6) 0.0234(2) Uani 1 d . .
C111 C 0.1060(3) 0.9016(2) 0.3793(2) 0.0266(7) Uani 1 d . .
H111 H 0.0614 0.908 0.4355 0.032 Uiso 1 calc . .
C112 C 0.1956(3) 0.9724(3) 0.3679(3) 0.0337(9) Uani 1 d . .
H11A H 0.246 0.9535 0.4109 0.04 Uiso 1 calc . .
H11B H 0.237 0.9747 0.3099 0.04 Uiso 1 calc . .
C113 C 0.1443(4) 1.0683(3) 0.3794(3) 0.0480(12) Uani 1 d . .
H11C H 0.1072 1.0665 0.4389 0.058 Uiso 1 calc . .
H11D H 0.2016 1.1142 0.3708 0.058 Uiso 1 calc . .
C114 C 0.0635(4) 1.0984(3) 0.3159(4) 0.0533(13) Uani 1 d . .
H11E H 0.0266 1.1574 0.3289 0.064 Uiso 1 calc . .
H11F H 0.1027 1.1098 0.257 0.064 Uiso 1 calc . .
C115 C -0.0205(4) 1.0261(3) 0.3192(3) 0.0454(11) Uani 1 d . .
H11G H -0.0658 1.0454 0.2726 0.054 Uiso 1 calc . .
H11H H -0.0681 1.0225 0.3747 0.054 Uiso 1 calc . .
C116 C 0.0315(3) 0.9301(3) 0.3096(3) 0.0367(9) Uani 1 d . .
H11I H 0.0737 0.9316 0.2519 0.044 Uiso 1 calc . .
H11J H -0.0253 0.8841 0.3152 0.044 Uiso 1 calc . .
C121 C 0.0263(3) 0.7186(2) 0.3949(2) 0.0248(7) Uani 1 d . .
H121 H -0.0011 0.7386 0.3383 0.03 Uiso 1 calc . .
C122 C 0.0386(3) 0.6128(3) 0.4030(3) 0.0304(8) Uani 1 d . .
H12A H 0.0972 0.5952 0.3593 0.036 Uiso 1 calc . .
H12B H 0.0581 0.5873 0.4605 0.036 Uiso 1 calc . .
C123 C -0.0672(3) 0.5722(3) 0.3901(3) 0.0320(8) Uani 1 d . .
H12C H -0.0839 0.5948 0.3311 0.038 Uiso 1 calc . .
H12D H -0.0586 0.5037 0.3964 0.038 Uiso 1 calc . .
C124 C -0.1604(3) 0.5992(3) 0.4547(3) 0.0366(9) Uani 1 d . .
H12E H -0.1481 0.5701 0.5133 0.044 Uiso 1 calc . .
H12F H -0.2283 0.5758 0.4418 0.044 Uiso 1 calc . .
C125 C -0.1712(3) 0.7041(3) 0.4517(3) 0.0412(10) Uani 1 d . .
H12G H -0.2276 0.7193 0.4981 0.049 Uiso 1 calc . .
H12H H -0.1944 0.7323 0.396 0.049 Uiso 1 calc . .
C126 C -0.0651(3) 0.7454(3) 0.4623(3) 0.0387(10) Uani 1 d . .
H12I H -0.046 0.7227 0.5206 0.046 Uiso 1 calc . .
H12J H -0.0741 0.8138 0.4564 0.046 Uiso 1 calc . .
C131 C 0.2216(10) 0.7543(9) 0.4870(8) 0.027(3) Uani 0.5 d A 1
H131 H 0.2984 0.7722 0.4705 0.032 Uiso 0.5 calc A 1
C132 C 0.1746(9) 0.8100(7) 0.5584(6) 0.037(2) Uani 0.5 d A 1
H13A H 0.1 0.7911 0.5803 0.045 Uiso 0.5 calc A 1
H13B H 0.1721 0.8769 0.5354 0.045 Uiso 0.5 calc A 1
C133 C 0.245(3) 0.7927(12) 0.6321(12) 0.0354(17) Uani 0.5 d A 1
H13C H 0.318 0.8162 0.6107 0.042 Uiso 0.5 calc A 1
H13D H 0.2132 0.8275 0.6789 0.042 Uiso 0.5 calc A 1
C134 C 0.2548(12) 0.6904(10) 0.6673(8) 0.045(3) Uani 0.5 d A 1
H13E H 0.3053 0.6815 0.7111 0.053 Uiso 0.5 calc A 1
H13F H 0.1834 0.6688 0.6956 0.053 Uiso 0.5 calc A 1
C135 C 0.2952(17) 0.6334(12) 0.5965(11) 0.051(6) Uani 0.5 d A 1
H13G H 0.2953 0.5667 0.6205 0.062 Uiso 0.5 calc A 1
H13H H 0.3704 0.6494 0.5732 0.062 Uiso 0.5 calc A 1
C136 C 0.2242(14) 0.6510(10) 0.5239(11) 0.028(4) Uani 0.5 d A 1
H13I H 0.15 0.6313 0.5462 0.033 Uiso 0.5 calc A 1
H13J H 0.2531 0.614 0.4779 0.033 Uiso 0.5 calc A 1
C141 C 0.1826(9) 0.7498(9) 0.5015(8) 0.025(3) Uani 0.5 d A 2
H141 H 0.1113 0.7351 0.5364 0.03 Uiso 0.5 calc A 2
C142 C 0.2279(9) 0.8252(6) 0.5408(6) 0.032(2) Uani 0.5 d A 2
H14A H 0.1808 0.882 0.5338 0.039 Uiso 0.5 calc A 2
H14B H 0.3005 0.8403 0.5104 0.039 Uiso 0.5 calc A 2
C143 C 0.235(3) 0.7943(12) 0.6369(11) 0.0354(17) Uani 0.5 d A 2
H14C H 0.2686 0.8435 0.6603 0.042 Uiso 0.5 calc A 2
H14D H 0.1619 0.7855 0.6681 0.042 Uiso 0.5 calc A 2
C144 C 0.3019(9) 0.7047(9) 0.6515(8) 0.036(3) Uani 0.5 d A 2
H14E H 0.3783 0.7162 0.6285 0.043 Uiso 0.5 calc A 2
H14F H 0.2983 0.6831 0.714 0.043 Uiso 0.5 calc A 2
C145 C 0.2618(15) 0.6302(11) 0.6082(12) 0.035(4) Uani 0.5 d A 2
H14G H 0.1899 0.6115 0.638 0.043 Uiso 0.5 calc A 2
H14H H 0.3116 0.5751 0.6139 0.043 Uiso 0.5 calc A 2
C146 C 0.2531(14) 0.6612(10) 0.5135(11) 0.029(4) Uani 0.5 d A 2
H14I H 0.2215 0.6116 0.4895 0.035 Uiso 0.5 calc A 2
H14J H 0.326 0.6725 0.4818 0.035 Uiso 0.5 calc A 2
C100 C 0.3031(7) 0.6314(6) 0.2809(6) 0.0180(18) Uani 0.5 d B 1
H100 H 0.2604 0.6002 0.2498 0.022 Uiso 0.5 calc B 1
C101 C 0.3719(6) 0.5674(5) 0.3366(5) 0.0227(16) Uani 0.5 d B 1
C102 C 0.4440(6) 0.5906(6) 0.3850(5) 0.0363(18) Uani 0.5 d B 1
H102 H 0.4609 0.6538 0.3816 0.044 Uiso 0.5 calc B 1
C103 C 0.4943(7) 0.5232(7) 0.4402(6) 0.049(2) Uani 0.5 d B 1
H103 H 0.5441 0.5407 0.4745 0.059 Uiso 0.5 calc B 1
C104 C 0.4716(7) 0.4312(7) 0.4446(6) 0.050(2) Uani 0.5 d B 1
H104 H 0.5057 0.3852 0.4822 0.06 Uiso 0.5 calc B 1
C105 C 0.4012(12) 0.4063(8) 0.3960(8) 0.053(3) Uani 0.5 d B 1
H105 H 0.3853 0.3427 0.4003 0.064 Uiso 0.5 calc B 1
C106 C 0.3511(8) 0.4715(6) 0.3393(7) 0.031(2) Uani 0.5 d B 1
H106 H 0.3042 0.4528 0.3033 0.038 Uiso 0.5 calc B 1
C200 C 0.3425(10) 0.6398(8) 0.3037(7) 0.039(2) Uani 0.5 d B 2
H200 H 0.406 0.6481 0.328 0.046 Uiso 0.5 calc B 2
C201 C 0.3258(8) 0.5452(7) 0.3124(6) 0.050(3) Uani 0.5 d B 2
C202 C 0.2409(8) 0.5087(6) 0.2808(7) 0.056(3) Uani 0.5 d B 2
H202 H 0.1938 0.5497 0.2495 0.068 Uiso 0.5 calc B 2
C203 C 0.2229(10) 0.4124(7) 0.2942(7) 0.071(3) Uani 0.5 d B 2
H203 H 0.1621 0.3881 0.2764 0.085 Uiso 0.5 calc B 2
C204 C 0.2987(9) 0.3551(7) 0.3348(7) 0.077(4) Uani 0.5 d B 2
H204 H 0.2918 0.2898 0.3409 0.092 Uiso 0.5 calc B 2
C205 C 0.3843(12) 0.3890(8) 0.3668(9) 0.053(3) Uani 0.5 d B 2
H205 H 0.4326 0.3478 0.3968 0.064 Uiso 0.5 calc B 2
C206 C 0.3982(11) 0.4842(8) 0.3543(10) 0.066(4) Uani 0.5 d B 2
H206 H 0.4577 0.5081 0.3744 0.08 Uiso 0.5 calc B 2
Cl11 Cl 0.57188(11) 0.88014(11) 0.55426(9) 0.0641(3) Uani 1 d . .
Cl12 Cl 0.70783(11) 0.95441(10) 0.39933(10) 0.0635(4) Uani 1 d . .
C10 C 0.5910(4) 0.8927(4) 0.4420(3) 0.0492(11) Uani 1 d . .
H10A H 0.5274 0.926 0.4194 0.059 Uiso 1 calc . .
H10B H 0.5975 0.8306 0.4233 0.059 Uiso 1 calc . .
Cl21 Cl 0.0887(3) 0.3679(2) 0.2786(3) 0.1030(14) Uani 0.5 d C 1
Cl22 Cl -0.0019(3) 0.4404(4) 0.1206(5) 0.120(2) Uani 0.5 d C 1
C20 C -0.0319(7) 0.4016(9) 0.2246(6) 0.069(3) Uiso 0.5 d C 1
H20A H -0.078 0.3474 0.2312 0.083 Uiso 0.5 calc C 1
H20B H -0.0739 0.4506 0.253 0.083 Uiso 0.5 calc C 1
Cl31 Cl 0.0061(5) 0.4912(9) 0.0387(5) 0.209(4) Uani 0.5 d D 2
Cl32 Cl 0.0676(12) 0.4639(9) 0.2056(9) 0.378(12) Uani 0.5 d D 2
C30 C -0.017(3) 0.424(3) 0.1425(13) 0.26(3) Uiso 0.5 d D 2
H30A H -0.0937 0.4315 0.1675 0.311 Uiso 0.5 calc D 2
H30B H -0.0013 0.3573 0.1386 0.311 Uiso 0.5 calc D 2



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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C100 1.819(9) . ?
Ru1 C200 1.877(11) . ?
Ru1 C1 2.086(3) . ?
Ru1 Cl2 2.3822(9) . ?
Ru1 Cl1 2.3882(9) . ?
Ru1 P1 2.4371(9) . ?
C1 N5 1.348(4) . ?
C1 N2 1.359(4) . ?
N2 C21 1.420(5) . ?
N2 C3 1.477(4) . ?
C21 C22 1.391(5) . ?
C21 C28A 1.417(5) . ?
C22 N221 1.404(5) . ?
C22 C23 1.422(6) . ?
N221 C226 1.460(6) . ?
N221 C222 1.469(5) . ?
C222 C223 1.513(8) . ?
C222 H22A 0.99 . ?
C222 H22B 0.99 . ?
C223 C224 1.508(9) . ?
C223 H22C 0.99 . ?
C223 H22D 0.99 . ?
C224 C225 1.542(7) . ?
C224 H22E 0.99 . ?
C224 H22F 0.99 . ?
C225 C226 1.511(7) . ?
C225 H22G 0.99 . ?
C225 H22H 0.99 . ?
C226 H22I 0.99 . ?
C226 H22J 0.99 . ?
C23 C2 1.348(7) . ?
C23 H23 0.95 . ?
C24A C2 1.409(7) . ?
C24A C25 1.413(7) . ?
C24A C28A 1.423(5) . ?
C25 C26 1.347(8) . ?
C25 H25 0.95 . ?
C26 C27 1.405(7) . ?
C26 H26 0.95 . ?
C27 C28 1.369(6) . ?
C27 H27 0.95 . ?
C28 C28A 1.413(6) . ?
C28 H28 0.95 . ?
C2 H2 0.95 . ?
C3 C4 1.507(5) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N5 1.476(5) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
N5 C51 1.430(5) . ?
C51 C52 1.381(6) . ?
C51 C58A 1.428(6) . ?
C52 N521 1.425(6) . ?
C52 C53 1.428(6) . ?
N521 C526 1.464(5) . ?
N521 C522 1.465(6) . ?
C522 C523 1.530(8) . ?
C522 H52A 0.99 . ?
C522 H52B 0.99 . ?
C523 C524 1.526(7) . ?
C523 H52C 0.99 . ?
C523 H52D 0.99 . ?
C524 C525 1.532(7) . ?
C524 H52E 0.99 . ?
C524 H52F 0.99 . ?
C525 C526 1.505(8) . ?
C525 H52G 0.99 . ?
C525 H52H 0.99 . ?
C526 H52I 0.99 . ?
C526 H52J 0.99 . ?
C53 C54 1.356(8) . ?
C53 H53 0.95 . ?
C54 C54A 1.402(7) . ?
C54 H54 0.95 . ?
C54A C58A 1.422(6) . ?
C54A C55 1.427(7) . ?
C55 C56 1.363(9) . ?
C55 H55 0.95 . ?
C56 C57 1.394(8) . ?
C56 H56 0.95 . ?
C57 C58 1.372(6) . ?
C57 H57 0.95 . ?
C58 C58A 1.414(6) . ?
C58 H58 0.95 . ?
P1 C121 1.855(4) . ?
P1 C111 1.858(4) . ?
P1 C131 1.876(14) . ?
P1 C141 1.885(13) . ?
C111 C116 1.537(5) . ?
C111 C112 1.541(5) . ?
C111 H111 1 . ?
C112 C113 1.532(5) . ?
C112 H11A 0.99 . ?
C112 H11B 0.99 . ?
C113 C114 1.524(7) . ?
C113 H11C 0.99 . ?
C113 H11D 0.99 . ?
C114 C115 1.521(6) . ?
C114 H11E 0.99 . ?
C114 H11F 0.99 . ?
C115 C116 1.531(5) . ?
C115 H11G 0.99 . ?
C115 H11H 0.99 . ?
C116 H11I 0.99 . ?
C116 H11J 0.99 . ?
C121 C122 1.530(5) . ?
C121 C126 1.533(5) . ?
C121 H121 1 . ?
C122 C123 1.530(5) . ?
C122 H12A 0.99 . ?
C122 H12B 0.99 . ?
C123 C124 1.520(6) . ?
C123 H12C 0.99 . ?
C123 H12D 0.99 . ?
C124 C125 1.522(6) . ?
C124 H12E 0.99 . ?
C124 H12F 0.99 . ?
C125 C126 1.528(6) . ?
C125 H12G 0.99 . ?
C125 H12H 0.99 . ?
C126 H12I 0.99 . ?
C126 H12J 0.99 . ?
C131 C132 1.527(11) . ?
C131 C136 1.534(12) . ?
C131 H131 1 . ?
C132 C133 1.540(14) . ?
C132 H13A 0.99 . ?
C132 H13B 0.99 . ?
C133 C134 1.517(14) . ?
C133 H13C 0.99 . ?
C133 H13D 0.99 . ?
C134 C135 1.513(13) . ?
C134 H13E 0.99 . ?
C134 H13F 0.99 . ?
C135 C136 1.530(12) . ?
C135 H13G 0.99 . ?
C135 H13H 0.99 . ?
C136 H13I 0.99 . ?
C136 H13J 0.99 . ?
C141 C142 1.514(11) . ?
C141 C146 1.525(12) . ?
C141 H141 1 . ?
C142 C143 1.536(14) . ?
C142 H14A 0.99 . ?
C142 H14B 0.99 . ?
C143 C144 1.515(14) . ?
C143 H14C 0.99 . ?
C143 H14D 0.99 . ?
C144 C145 1.511(13) . ?
C144 H14E 0.99 . ?
C144 H14F 0.99 . ?
C145 C146 1.519(13) . ?
C145 H14G 0.99 . ?
C145 H14H 0.99 . ?
C146 H14I 0.99 . ?
C146 H14J 0.99 . ?
C100 C101 1.503(11) . ?
C100 H100 0.95 . ?
C101 C102 1.349(11) . ?
C101 C106 1.429(10) . ?
C102 C103 1.396(10) . ?
C102 H102 0.95 . ?
C103 C104 1.376(12) . ?
C103 H103 0.95 . ?
C104 C105 1.343(14) . ?
C104 H104 0.95 . ?
C105 C106 1.390(12) . ?
C105 H105 0.95 . ?
C106 H106 0.95 . ?
C200 C201 1.391(15) . ?
C200 H200 0.95 . ?
C201 C206 1.395(8) . ?
C201 C202 1.396(8) . ?
C202 C203 1.416(8) . ?
C202 H202 0.95 . ?
C203 C204 1.388(8) . ?
C203 H203 0.95 . ?
C204 C205 1.390(9) . ?
C204 H204 0.95 . ?
C205 C206 1.391(8) . ?
C205 H205 0.95 . ?
C206 H206 0.95 . ?
Cl11 C10 1.747(5) . ?
Cl12 C10 1.761(5) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
Cl21 C20 1.842(7) . ?
Cl22 C20 1.660(7) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
Cl31 C30 1.784(8) . ?
Cl32 C30 1.734(8) . ?
C30 H30A 0.99 . ?
C30 H30B 0.99 . ?

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
C100 Ru1 C1 98.6(3) . . ?
C200 Ru1 C1 98.4(3) . . ?
C100 Ru1 Cl2 84.4(3) . . ?
C200 Ru1 Cl2 105.3(4) . . ?
C1 Ru1 Cl2 93.39(9) . . ?
C100 Ru1 Cl1 107.5(3) . . ?
C200 Ru1 Cl1 86.5(4) . . ?
C1 Ru1 Cl1 87.74(9) . . ?
Cl2 Ru1 Cl1 167.84(4) . . ?
C100 Ru1 P1 99.0(3) . . ?
C200 Ru1 P1 98.1(3) . . ?
C1 Ru1 P1 162.44(10) . . ?
Cl2 Ru1 P1 88.19(3) . . ?
Cl1 Ru1 P1 87.15(3) . . ?
N5 C1 N2 106.0(3) . . ?
N5 C1 Ru1 124.0(2) . . ?
N2 C1 Ru1 129.5(2) . . ?
C1 N2 C21 129.0(3) . . ?
C1 N2 C3 112.2(3) . . ?
C21 N2 C3 116.5(3) . . ?
C22 C21 C28A 121.1(3) . . ?
C22 C21 N2 118.8(3) . . ?
C28A C21 N2 118.5(3) . . ?
C21 C22 N221 120.9(3) . . ?
C21 C22 C23 117.7(4) . . ?
N221 C22 C23 121.1(4) . . ?
C22 N221 C226 119.3(3) . . ?
C22 N221 C222 117.7(4) . . ?
C226 N221 C222 111.8(4) . . ?
N221 C222 C223 108.9(4) . . ?
N221 C222 H22A 109.9 . . ?
C223 C222 H22A 109.9 . . ?
N221 C222 H22B 109.9 . . ?
C223 C222 H22B 109.9 . . ?
H22A C222 H22B 108.3 . . ?
C224 C223 C222 112.7(4) . . ?
C224 C223 H22C 109.1 . . ?
C222 C223 H22C 109.1 . . ?
C224 C223 H22D 109.1 . . ?
C222 C223 H22D 109.1 . . ?
H22C C223 H22D 107.8 . . ?
C223 C224 C225 110.6(4) . . ?
C223 C224 H22E 109.5 . . ?
C225 C224 H22E 109.5 . . ?
C223 C224 H22F 109.5 . . ?
C225 C224 H22F 109.5 . . ?
H22E C224 H22F 108.1 . . ?
C226 C225 C224 111.1(5) . . ?
C226 C225 H22G 109.4 . . ?
C224 C225 H22G 109.4 . . ?
C226 C225 H22H 109.4 . . ?
C224 C225 H22H 109.4 . . ?
H22G C225 H22H 108 . . ?
N221 C226 C225 110.0(4) . . ?
N221 C226 H22I 109.7 . . ?
C225 C226 H22I 109.7 . . ?
N221 C226 H22J 109.7 . . ?
C225 C226 H22J 109.7 . . ?
H22I C226 H22J 108.2 . . ?
C2 C23 C22 121.7(4) . . ?
C2 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C2 C24A C25 122.5(4) . . ?
C2 C24A C28A 118.4(4) . . ?
C25 C24A C28A 119.0(4) . . ?
C26 C25 C24A 121.5(4) . . ?
C26 C25 H25 119.2 . . ?
C24A C25 H25 119.2 . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120 . . ?
C27 C26 H26 120 . . ?
C28 C27 C26 120.4(5) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C28A 121.1(4) . . ?
C27 C28 H28 119.5 . . ?
C28A C28 H28 119.5 . . ?
C28 C28A C21 123.0(3) . . ?
C28 C28A C24A 118.0(4) . . ?
C21 C28A C24A 119.0(4) . . ?
C23 C2 C24A 121.4(4) . . ?
C23 C2 H2 119.3 . . ?
C24A C2 H2 119.3 . . ?
N2 C3 C4 101.9(3) . . ?
N2 C3 H3A 111.4 . . ?
C4 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C4 C3 H3B 111.4 . . ?
H3A C3 H3B 109.3 . . ?
N5 C4 C3 100.7(3) . . ?
N5 C4 H4A 111.6 . . ?
C3 C4 H4A 111.6 . . ?
N5 C4 H4B 111.6 . . ?
C3 C4 H4B 111.6 . . ?
H4A C4 H4B 109.4 . . ?
C1 N5 C51 128.2(3) . . ?
C1 N5 C4 113.3(3) . . ?
C51 N5 C4 118.3(3) . . ?
C52 C51 C58A 121.8(4) . . ?
C52 C51 N5 119.4(4) . . ?
C58A C51 N5 118.2(3) . . ?
C51 C52 N521 120.8(4) . . ?
C51 C52 C53 117.7(4) . . ?
N521 C52 C53 121.5(4) . . ?
C52 N521 C526 115.4(4) . . ?
C52 N521 C522 114.5(4) . . ?
C526 N521 C522 110.3(3) . . ?
N521 C522 C523 110.2(4) . . ?
N521 C522 H52A 109.6 . . ?
C523 C522 H52A 109.6 . . ?
N521 C522 H52B 109.6 . . ?
C523 C522 H52B 109.6 . . ?
H52A C522 H52B 108.1 . . ?
C524 C523 C522 109.8(5) . . ?
C524 C523 H52C 109.7 . . ?
C522 C523 H52C 109.7 . . ?
C524 C523 H52D 109.7 . . ?
C522 C523 H52D 109.7 . . ?
H52C C523 H52D 108.2 . . ?
C523 C524 C525 109.3(4) . . ?
C523 C524 H52E 109.8 . . ?
C525 C524 H52E 109.8 . . ?
C523 C524 H52F 109.8 . . ?
C525 C524 H52F 109.8 . . ?
H52E C524 H52F 108.3 . . ?
C526 C525 C524 112.3(4) . . ?
C526 C525 H52G 109.2 . . ?
C524 C525 H52G 109.2 . . ?
C526 C525 H52H 109.2 . . ?
C524 C525 H52H 109.2 . . ?
H52G C525 H52H 107.9 . . ?
N521 C526 C525 110.0(4) . . ?
N521 C526 H52I 109.7 . . ?
C525 C526 H52I 109.7 . . ?
N521 C526 H52J 109.7 . . ?
C525 C526 H52J 109.7 . . ?
H52I C526 H52J 108.2 . . ?
C54 C53 C52 121.6(4) . . ?
C54 C53 H53 119.2 . . ?
C52 C53 H53 119.2 . . ?
C53 C54 C54A 121.4(4) . . ?
C53 C54 H54 119.3 . . ?
C54A C54 H54 119.3 . . ?
C54 C54A C58A 118.9(4) . . ?
C54 C54A C55 122.5(4) . . ?
C58A C54A C55 118.5(5) . . ?
C56 C55 C54A 121.2(5) . . ?
C56 C55 H55 119.4 . . ?
C54A C55 H55 119.4 . . ?
C55 C56 C57 119.8(5) . . ?
C55 C56 H56 120.1 . . ?
C57 C56 H56 120.1 . . ?
C58 C57 C56 121.1(5) . . ?
C58 C57 H57 119.5 . . ?
C56 C57 H57 119.5 . . ?
C57 C58 C58A 120.7(4) . . ?
C57 C58 H58 119.7 . . ?
C58A C58 H58 119.7 . . ?
C58 C58A C54A 118.6(4) . . ?
C58 C58A C51 122.9(4) . . ?
C54A C58A C51 118.4(4) . . ?
C121 P1 C111 101.07(16) . . ?
C121 P1 C131 113.2(4) . . ?
C111 P1 C131 105.6(4) . . ?
C121 P1 C141 99.2(4) . . ?
C111 P1 C141 102.8(4) . . ?
C121 P1 Ru1 115.86(11) . . ?
C111 P1 Ru1 110.12(12) . . ?
C131 P1 Ru1 110.1(3) . . ?
C141 P1 Ru1 124.6(4) . . ?
C116 C111 C112 109.0(3) . . ?
C116 C111 P1 113.4(3) . . ?
C112 C111 P1 114.7(3) . . ?
C116 C111 H111 106.4 . . ?
C112 C111 H111 106.4 . . ?
P1 C111 H111 106.4 . . ?
C113 C112 C111 109.2(3) . . ?
C113 C112 H11A 109.8 . . ?
C111 C112 H11A 109.8 . . ?
C113 C112 H11B 109.8 . . ?
C111 C112 H11B 109.8 . . ?
H11A C112 H11B 108.3 . . ?
C114 C113 C112 111.3(4) . . ?
C114 C113 H11C 109.4 . . ?
C112 C113 H11C 109.4 . . ?
C114 C113 H11D 109.4 . . ?
C112 C113 H11D 109.4 . . ?
H11C C113 H11D 108 . . ?
C115 C114 C113 112.3(4) . . ?
C115 C114 H11E 109.1 . . ?
C113 C114 H11E 109.1 . . ?
C115 C114 H11F 109.1 . . ?
C113 C114 H11F 109.1 . . ?
H11E C114 H11F 107.9 . . ?
C114 C115 C116 111.9(4) . . ?
C114 C115 H11G 109.2 . . ?
C116 C115 H11G 109.2 . . ?
C114 C115 H11H 109.2 . . ?
C116 C115 H11H 109.2 . . ?
H11G C115 H11H 107.9 . . ?
C115 C116 C111 109.5(3) . . ?
C115 C116 H11I 109.8 . . ?
C111 C116 H11I 109.8 . . ?
C115 C116 H11J 109.8 . . ?
C111 C116 H11J 109.8 . . ?
H11I C116 H11J 108.2 . . ?
C122 C121 C126 109.3(3) . . ?
C122 C121 P1 114.5(2) . . ?
C126 C121 P1 116.8(3) . . ?
C122 C121 H121 105 . . ?
C126 C121 H121 105 . . ?
P1 C121 H121 105 . . ?
C123 C122 C121 110.1(3) . . ?
C123 C122 H12A 109.7 . . ?
C121 C122 H12A 109.7 . . ?
C123 C122 H12B 109.7 . . ?
C121 C122 H12B 109.7 . . ?
H12A C122 H12B 108.2 . . ?
C124 C123 C122 111.6(3) . . ?
C124 C123 H12C 109.3 . . ?
C122 C123 H12C 109.3 . . ?
C124 C123 H12D 109.3 . . ?
C122 C123 H12D 109.3 . . ?
H12C C123 H12D 108 . . ?
C123 C124 C125 111.1(3) . . ?
C123 C124 H12E 109.4 . . ?
C125 C124 H12E 109.4 . . ?
C123 C124 H12F 109.4 . . ?
C125 C124 H12F 109.4 . . ?
H12E C124 H12F 108 . . ?
C124 C125 C126 111.8(4) . . ?
C124 C125 H12G 109.3 . . ?
C126 C125 H12G 109.3 . . ?
C124 C125 H12H 109.3 . . ?
C126 C125 H12H 109.3 . . ?
H12G C125 H12H 107.9 . . ?
C125 C126 C121 111.1(3) . . ?
C125 C126 H12I 109.4 . . ?
C121 C126 H12I 109.4 . . ?
C125 C126 H12J 109.4 . . ?
C121 C126 H12J 109.4 . . ?
H12I C126 H12J 108 . . ?
C132 C131 C136 108.8(10) . . ?
C132 C131 P1 115.1(8) . . ?
C136 C131 P1 112.6(9) . . ?
C132 C131 H131 106.6 . . ?
C136 C131 H131 106.6 . . ?
P1 C131 H131 106.6 . . ?
C131 C132 C133 109.6(11) . . ?
C131 C132 H13A 109.7 . . ?
C133 C132 H13A 109.7 . . ?
C131 C132 H13B 109.7 . . ?
C133 C132 H13B 109.7 . . ?
H13A C132 H13B 108.2 . . ?
C134 C133 C132 111.7(14) . . ?
C134 C133 H13C 109.3 . . ?
C132 C133 H13C 109.3 . . ?
C134 C133 H13D 109.3 . . ?
C132 C133 H13D 109.3 . . ?
H13C C133 H13D 107.9 . . ?
C135 C134 C133 111.2(12) . . ?
C135 C134 H13E 109.4 . . ?
C133 C134 H13E 109.4 . . ?
C135 C134 H13F 109.4 . . ?
C133 C134 H13F 109.4 . . ?
H13E C134 H13F 108 . . ?
C134 C135 C136 111.1(12) . . ?
C134 C135 H13G 109.4 . . ?
C136 C135 H13G 109.4 . . ?
C134 C135 H13H 109.4 . . ?
C136 C135 H13H 109.4 . . ?
H13G C135 H13H 108 . . ?
C135 C136 C131 110.2(12) . . ?
C135 C136 H13I 109.6 . . ?
C131 C136 H13I 109.6 . . ?
C135 C136 H13J 109.6 . . ?
C131 C136 H13J 109.6 . . ?
H13I C136 H13J 108.1 . . ?
C142 C141 C146 110.0(10) . . ?
C142 C141 P1 117.3(8) . . ?
C146 C141 P1 110.5(9) . . ?
C142 C141 H141 106.1 . . ?
C146 C141 H141 106.1 . . ?
P1 C141 H141 106.1 . . ?
C141 C142 C143 111.0(11) . . ?
C141 C142 H14A 109.4 . . ?
C143 C142 H14A 109.4 . . ?
C141 C142 H14B 109.4 . . ?
C143 C142 H14B 109.4 . . ?
H14A C142 H14B 108 . . ?
C144 C143 C142 111.5(13) . . ?
C144 C143 H14C 109.3 . . ?
C142 C143 H14C 109.3 . . ?
C144 C143 H14D 109.3 . . ?
C142 C143 H14D 109.3 . . ?
H14C C143 H14D 108 . . ?
C145 C144 C143 111.4(12) . . ?
C145 C144 H14E 109.4 . . ?
C143 C144 H14E 109.4 . . ?
C145 C144 H14F 109.4 . . ?
C143 C144 H14F 109.4 . . ?
H14E C144 H14F 108 . . ?
C144 C145 C146 113.0(12) . . ?
C144 C145 H14G 109 . . ?
C146 C145 H14G 109 . . ?
C144 C145 H14H 109 . . ?
C146 C145 H14H 109 . . ?
H14G C145 H14H 107.8 . . ?
C145 C146 C141 110.6(12) . . ?
C145 C146 H14I 109.5 . . ?
C141 C146 H14I 109.5 . . ?
C145 C146 H14J 109.5 . . ?
C141 C146 H14J 109.5 . . ?
H14I C146 H14J 108.1 . . ?
C101 C100 Ru1 132.4(7) . . ?
C101 C100 H100 113.8 . . ?
Ru1 C100 H100 113.8 . . ?
C102 C101 C106 118.8(7) . . ?
C102 C101 C100 127.8(7) . . ?
C106 C101 C100 113.3(8) . . ?
C101 C102 C103 121.0(8) . . ?
C101 C102 H102 119.5 . . ?
C103 C102 H102 119.5 . . ?
C104 C103 C102 119.9(9) . . ?
C104 C103 H103 120 . . ?
C102 C103 H103 120 . . ?
C103 C103 H103 52.6 2_666 . ?
C105 C104 C103 120.0(9) . . ?
C105 C104 H104 120 . . ?
C103 C104 H104 120 . . ?
C104 C105 C106 121.5(11) . . ?
C104 C105 H105 119.2 . . ?
C106 C105 H105 119.2 . . ?
C105 C106 C101 118.5(9) . . ?
C105 C106 H106 120.7 . . ?
C101 C106 H106 120.7 . . ?
C201 C200 Ru1 143.3(11) . . ?
C201 C200 H200 108.3 . . ?
Ru1 C200 H200 108.3 . . ?
C200 C201 C206 118.1(10) . . ?
C200 C201 C202 123.1(10) . . ?
C206 C201 C202 118.8(10) . . ?
C201 C202 C203 121.8(10) . . ?
C201 C202 H202 119.1 . . ?
C203 C202 H202 119.1 . . ?
C204 C203 C202 116.6(10) . . ?
C204 C203 H203 121.7 . . ?
C202 C203 H203 121.7 . . ?
C203 C204 C205 122.9(10) . . ?
C203 C204 H204 118.6 . . ?
C205 C204 H204 118.6 . . ?
C204 C205 C206 118.9(11) . . ?
C204 C205 H205 120.6 . . ?
C206 C205 H205 120.6 . . ?
C205 C206 C201 120.8(11) . . ?
C205 C206 H206 119.6 . . ?
C201 C206 H206 119.6 . . ?
Cl11 C10 Cl12 111.2(3) . . ?
Cl11 C10 H10A 109.4 . . ?
Cl12 C10 H10A 109.4 . . ?
Cl11 C10 H10B 109.4 . . ?
Cl12 C10 H10B 109.4 . . ?
H10A C10 H10B 108 . . ?
Cl22 C20 Cl21 112.9(6) . . ?
Cl22 C20 H20A 109 . . ?
Cl21 C20 H20A 109 . . ?
Cl22 C20 H20B 109 . . ?
Cl21 C20 H20B 109 . . ?
H20A C20 H20B 107.8 . . ?
Cl32 C30 Cl31 106.7(10) . . ?
Cl32 C30 H30A 110.4 . . ?
Cl31 C30 H30A 110.4 . . ?
Cl32 C30 H30B 110.4 . . ?
Cl31 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?

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

data_rda609
_database_code_depnum_ccdc_archive 'CCDC 1518964'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT094_rda609              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       7.36 Report         
          
RESPONSE: 
The largest peak in the difference map is 1.45 Angstroms from H14A; the
deepest hole is 1.87 Angstroms from H21F.
;


_vrf_PLAT930_rda609              
;
PROBLEM: Check Twin Law ( 1-1  0)[ 5-2  1] Estimated BASF       0.17          
          
RESPONSE: 
Refined as a 2-component twin.
;

_audit_creation_date             2016-01-19T11:27:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C39 H44 Cl Ir N4 O2'
_chemical_formula_moiety         'C39 H44 Cl Ir N4 O2'
_chemical_formula_weight         828.43

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

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

_cell_length_a                   13.0670(3)
_cell_length_b                   16.7164(5)
_cell_length_c                   16.8853(4)
_cell_angle_alpha                94.087(2)
_cell_angle_beta                 109.624(2)
_cell_angle_gamma                104.374(3)
_cell_volume                     3316.64(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21724
_cell_measurement_theta_min      2.012
_cell_measurement_theta_max      34.132

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

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.121
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.0744
0 0 1 0.1508
-1 1 0 0.0622
1 -1 0 0.0588
1 1 -2 0.0815
-2 -3 2 0.0985
0 2 1 0.2025
0 -2 3 0.1246
0 -2 -3 0.2164
-2 1 5 0.1567


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

_exptl_absorpt_coefficient_mu    4.148
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
         CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)

;
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_correction_T_max  0.639

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

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0306622
_diffrn_orient_matrix_ub_12      -0.0280304
_diffrn_orient_matrix_ub_13      0.0178424
_diffrn_orient_matrix_ub_21      0.0512233
_diffrn_orient_matrix_ub_22      0.0290759
_diffrn_orient_matrix_ub_23      0.0024322
_diffrn_orient_matrix_ub_31      0.0078356
_diffrn_orient_matrix_ub_32      0.018555
_diffrn_orient_matrix_ub_33      0.0415149
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.047
_diffrn_reflns_number            34204
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.986
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_number_total             11670
_reflns_number_gt                10782
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


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

_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refined as a 2-component twin.
One morpholine group was found to be disordered over two sets of sites
 with site occupancies constrained to 0.5 after trial refinement.
The largest peak in the difference map is 1.45 Angstroms from H14A; the
deepest hole is 1.87 Angstroms from H21F.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0882P)²+17.9994P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11670
_refine_ls_number_parameters     884
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1308
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         7.676
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.195

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.61861(2) 0.79476(2) 1.00488(2) 0.01649(9) Uani 1 d . .
Ir2 Ir 0.13530(2) 0.30640(2) 0.43900(2) 0.01679(9) Uani 1 d . .
Cl1 Cl 0.73926(13) 0.71959(9) 1.08284(9) 0.0217(3) Uani 1 d . .
Cl2 Cl 0.28485(13) 0.25848(10) 0.42386(9) 0.0241(3) Uani 1 d . .
C111 C 0.4793(5) 0.8401(4) 0.9396(4) 0.0220(13) Uani 1 d . .
H111 H 0.4746 0.8086 0.8888 0.026 Uiso 1 calc . .
C112 C 0.5800(5) 0.9079(4) 0.9826(4) 0.0200(13) Uani 1 d . .
H112 H 0.634 0.9192 0.9558 0.024 Uiso 1 calc . .
C113 C 0.6094(6) 0.9636(4) 1.0669(4) 0.0248(14) Uani 1 d . .
H11A H 0.6923 0.9913 1.0911 0.03 Uiso 1 calc . .
H11B H 0.5708 1.0079 1.0564 0.03 Uiso 1 calc . .
C114 C 0.5751(6) 0.9154(4) 1.1310(4) 0.0276(14) Uani 1 d . .
H11C H 0.6201 0.9472 1.1894 0.033 Uiso 1 calc . .
H11D H 0.4939 0.9086 1.1202 0.033 Uiso 1 calc . .
C115 C 0.5947(6) 0.8303(4) 1.1243(4) 0.0240(14) Uani 1 d . .
H115 H 0.6693 0.8274 1.1539 0.029 Uiso 1 calc . .
C116 C 0.5133(6) 0.7561(4) 1.0787(4) 0.0241(14) Uani 1 d . .
H116 H 0.5368 0.7066 1.0811 0.029 Uiso 1 calc . .
C117 C 0.3905(6) 0.7464(5) 1.0253(5) 0.0339(17) Uani 1 d . .
H11E H 0.348 0.7499 1.0635 0.041 Uiso 1 calc . .
H11F H 0.3566 0.6904 0.9889 0.041 Uiso 1 calc . .
C118 C 0.3785(6) 0.8140(4) 0.9685(5) 0.0272(14) Uani 1 d . .
H11G H 0.3077 0.7923 0.9178 0.033 Uiso 1 calc . .
H11H H 0.373 0.8637 1.0006 0.033 Uiso 1 calc . .
C11 C 0.6699(5) 0.7783(4) 0.9028(4) 0.0154(12) Uani 1 d . .
N12 N 0.7227(4) 0.8364(3) 0.8659(3) 0.0160(10) Uani 1 d . .
C121 C 0.7589(5) 0.9259(4) 0.8901(4) 0.0174(12) Uani 1 d . .
C122 C 0.7203(5) 0.9745(4) 0.8304(4) 0.0195(13) Uani 1 d . .
C123 C 0.7497(6) 1.0624(4) 0.8557(4) 0.0236(13) Uani 1 d . .
H123 H 0.724 1.096 0.8147 0.028 Uiso 1 calc . .
C124 C 0.8139(6) 1.0993(4) 0.9376(4) 0.0251(14) Uani 1 d . .
H124 H 0.8293 1.1579 0.9539 0.03 Uiso 1 calc . .
C125 C 0.9291(5) 1.0933(4) 1.0849(4) 0.0244(14) Uani 1 d . .
H125 H 0.9458 1.152 1.1012 0.029 Uiso 1 calc . .
C126 C 0.9720(6) 1.0425(4) 1.1434(4) 0.0277(15) Uani 1 d . .
H126 H 1.0166 1.0673 1.2011 0.033 Uiso 1 calc . .
C127 C 0.9502(6) 0.9556(4) 1.1181(4) 0.0254(14) Uani 1 d . .
H127 H 0.9834 0.9237 1.1583 0.03 Uiso 1 calc . .
C128 C 0.8827(5) 0.9170(4) 1.0371(4) 0.0192(12) Uani 1 d . .
H128 H 0.8676 0.8583 1.0216 0.023 Uiso 1 calc . .
C129 C 0.8584(5) 1.0509(4) 0.9992(4) 0.0221(13) Uani 1 d . .
C120 C 0.8344(5) 0.9641(4) 0.9755(4) 0.0181(12) Uani 1 d . .
N131 N 0.6484(5) 0.9359(3) 0.7444(3) 0.0231(11) Uani 1 d . .
C132 C 0.5274(6) 0.9085(5) 0.7320(5) 0.0373(18) Uani 1 d . .
H13A H 0.5004 0.9578 0.7395 0.045 Uiso 1 calc . .
H13B H 0.5158 0.8731 0.7746 0.045 Uiso 1 calc . .
C133 C 0.4620(7) 0.8592(6) 0.6433(5) 0.046(2) Uani 1 d . .
H13C H 0.4885 0.8093 0.6371 0.055 Uiso 1 calc . .
H13D H 0.3805 0.8394 0.6347 0.055 Uiso 1 calc . .
O134 O 0.4755(4) 0.9074(3) 0.5803(3) 0.0338(12) Uani 1 d . .
C135 C 0.5931(6) 0.9337(5) 0.5915(4) 0.0343(16) Uani 1 d . .
H13E H 0.6033 0.9675 0.5475 0.041 Uiso 1 calc . .
H13F H 0.6195 0.884 0.5846 0.041 Uiso 1 calc . .
C136 C 0.6628(6) 0.9852(5) 0.6792(4) 0.0306(16) Uani 1 d . .
H13G H 0.7439 1.0032 0.6862 0.037 Uiso 1 calc . .
H13H H 0.6384 1.0361 0.6854 0.037 Uiso 1 calc . .
C13 C 0.7614(6) 0.7980(4) 0.8034(4) 0.0222(13) Uani 1 d . .
H13I H 0.8435 0.8034 0.8283 0.027 Uiso 1 calc . .
H13J H 0.7454 0.8235 0.751 0.027 Uiso 1 calc . .
C14 C 0.6907(6) 0.7079(4) 0.7857(4) 0.0219(13) Uani 1 d . .
H14A H 0.623 0.6957 0.7325 0.026 Uiso 1 calc . .
H14B H 0.7355 0.669 0.7817 0.026 Uiso 1 calc . .
N15 N 0.6587(4) 0.7031(3) 0.8617(3) 0.0165(10) Uani 1 d . .
C151 C 0.6038(6) 0.6232(4) 0.8767(4) 0.0207(13) Uani 1 d . .
C152 C 0.6628(6) 0.5643(4) 0.8999(4) 0.0221(13) Uani 1 d . .
C153 C 0.6022(6) 0.4874(4) 0.9145(4) 0.0280(15) Uani 1 d . .
H153 H 0.6404 0.4463 0.9308 0.034 Uiso 1 calc . .
C154 C 0.4915(7) 0.4704(4) 0.9060(4) 0.0305(16) Uani 1 d . .
H154 H 0.4559 0.4194 0.92 0.037 Uiso 1 calc . .
C155 C 0.3135(6) 0.5094(4) 0.8666(4) 0.0306(16) Uani 1 d . .
H155 H 0.2767 0.4593 0.8812 0.037 Uiso 1 calc . .
C156 C 0.2536(6) 0.5639(5) 0.8359(5) 0.0345(17) Uani 1 d . .
H156 H 0.1768 0.5529 0.8315 0.041 Uiso 1 calc . .
C157 C 0.3058(6) 0.6362(4) 0.8107(5) 0.0320(16) Uani 1 d . .
H157 H 0.2626 0.6721 0.7856 0.038 Uiso 1 calc . .
C158 C 0.4194(6) 0.6559(4) 0.8221(4) 0.0260(14) Uani 1 d . .
H158 H 0.4538 0.7052 0.8049 0.031 Uiso 1 calc . .
C159 C 0.4288(6) 0.5260(4) 0.8774(4) 0.0251(14) Uani 1 d . .
C150 C 0.4849(6) 0.6030(4) 0.8593(4) 0.0222(13) Uani 1 d . .
N141 N 0.7758(5) 0.5778(3) 0.9047(4) 0.0242(12) Uani 1 d . .
C142 C 0.8649(6) 0.6487(4) 0.9640(4) 0.0256(14) Uani 1 d . .
H14C H 0.8823 0.6369 1.023 0.031 Uiso 1 calc . .
H14D H 0.8383 0.6993 0.9608 0.031 Uiso 1 calc . .
C143 C 0.9711(7) 0.6647(5) 0.9429(6) 0.0382(18) Uani 1 d . .
H14E H 0.9545 0.6801 0.8854 0.046 Uiso 1 calc . .
H14F H 1.0307 0.7125 0.9843 0.046 Uiso 1 calc . .
O144 O 1.0125(4) 0.5932(3) 0.9452(3) 0.0353(12) Uani 1 d . .
C145 C 0.9250(8) 0.5232(6) 0.8884(6) 0.048(2) Uani 1 d . .
H14G H 0.9533 0.4734 0.8911 0.058 Uiso 1 calc . .
H14H H 0.9059 0.5349 0.8294 0.058 Uiso 1 calc . .
C146 C 0.8194(7) 0.5042(5) 0.9096(6) 0.041(2) Uani 1 d . .
H14I H 0.7611 0.4553 0.8689 0.049 Uiso 1 calc . .
H14J H 0.8369 0.4902 0.9678 0.049 Uiso 1 calc . .
C211 C 0.0668(6) 0.2976(5) 0.2999(4) 0.0283(15) Uani 1 d . .
H211 H 0.0949 0.2507 0.2966 0.034 Uiso 1 calc . .
C212 C 0.1448(6) 0.3756(4) 0.3366(4) 0.0258(14) Uani 1 d . .
H212 H 0.2223 0.3771 0.3528 0.031 Uiso 1 calc . .
C213 C 0.1235(7) 0.4581(5) 0.3543(5) 0.0388(18) Uani 1 d . .
H21A H 0.1036 0.4819 0.3011 0.047 Uiso 1 calc . .
H21B H 0.1938 0.4976 0.3965 0.047 Uiso 1 calc . .
C214 C 0.0266(6) 0.4487(4) 0.3891(4) 0.0290(15) Uani 1 d . .
H21C H 0.0351 0.503 0.4219 0.035 Uiso 1 calc . .
H21D H -0.0474 0.4326 0.3409 0.035 Uiso 1 calc . .
C215 C 0.0286(6) 0.3816(4) 0.4471(4) 0.0215(13) Uani 1 d . .
H215 H 0.0766 0.3991 0.5055 0.026 Uiso 1 calc . .
C216 C -0.0348(5) 0.2963(4) 0.4207(4) 0.0212(13) Uani 1 d . .
H216 H -0.0282 0.2619 0.4636 0.025 Uiso 1 calc . .
C217 C -0.1128(6) 0.2543(5) 0.3302(4) 0.0293(15) Uani 1 d . .
H21E H -0.1859 0.2676 0.3169 0.035 Uiso 1 calc . .
H21F H -0.1286 0.1927 0.3262 0.035 Uiso 1 calc . .
C218 C -0.0607(6) 0.2828(5) 0.2645(4) 0.0289(15) Uani 1 d . .
H21G H -0.0952 0.2395 0.2125 0.035 Uiso 1 calc . .
H21H H -0.0777 0.3352 0.2485 0.035 Uiso 1 calc . .
C21 C 0.1811(5) 0.2871(4) 0.5634(4) 0.0174(12) Uani 1 d . .
N22 N 0.2816(4) 0.3276(3) 0.6255(3) 0.0176(10) Uani 1 d . .
C221 C 0.3708(5) 0.3928(4) 0.6190(4) 0.0214(13) Uani 1 d . .
C222 C 0.4751(5) 0.3811(4) 0.6318(4) 0.0258(14) Uani 1 d . .
C223 C 0.5610(6) 0.4469(5) 0.6214(5) 0.0381(19) Uani 1 d . .
H223 H 0.6332 0.439 0.6295 0.046 Uiso 1 calc . .
C224 C 0.5425(6) 0.5195(5) 0.6006(5) 0.0377(19) Uani 1 d . .
H224 H 0.6001 0.5605 0.5911 0.045 Uiso 1 calc . .
C225 C 0.4190(7) 0.6125(5) 0.5727(5) 0.0369(19) Uani 1 d . .
H225 H 0.475 0.6535 0.5616 0.044 Uiso 1 calc . .
C226 C 0.3206(8) 0.6287(5) 0.5689(6) 0.044(2) Uani 1 d . .
H226 H 0.3071 0.6797 0.5534 0.053 Uiso 1 calc . .
C227 C 0.2389(7) 0.5691(4) 0.5883(5) 0.0372(18) Uani 1 d . .
H227 H 0.1724 0.5819 0.5892 0.045 Uiso 1 calc . .
C228 C 0.2541(6) 0.4930(4) 0.6058(4) 0.0294(15) Uani 1 d . .
H228 H 0.1981 0.4537 0.6187 0.035 Uiso 1 calc . .
C229 C 0.4399(6) 0.5359(4) 0.5927(4) 0.0327(17) Uani 1 d . .
C220 C 0.3530(6) 0.4728(4) 0.6047(4) 0.0255(14) Uani 1 d . .
N231 N 0.4991(5) 0.3054(5) 0.6570(4) 0.0349(15) Uani 0.5 d A 1
C232 C 0.6270(14) 0.3310(12) 0.7057(13) 0.046(4) Uani 0.5 d A 1
H23A H 0.6685 0.3318 0.6661 0.055 Uiso 0.5 calc A 1
H23B H 0.6536 0.3869 0.7417 0.055 Uiso 0.5 calc A 1
C233 C 0.6426(16) 0.2642(14) 0.7591(10) 0.046(5) Uani 0.5 d A 1
H23C H 0.5983 0.2634 0.7966 0.055 Uiso 0.5 calc A 1
H23D H 0.7237 0.2769 0.7958 0.055 Uiso 0.5 calc A 1
O234 O 0.6029(5) 0.1767(4) 0.7021(4) 0.0461(14) Uani 0.5 d A 1
C235 C 0.4763(13) 0.1704(11) 0.6651(11) 0.041(4) Uani 0.5 d A 1
H23E H 0.4333 0.114 0.6308 0.049 Uiso 0.5 calc A 1
H23F H 0.4488 0.1776 0.7124 0.049 Uiso 0.5 calc A 1
C236 C 0.4547(14) 0.2364(10) 0.6096(9) 0.035(3) Uani 0.5 d A 1
H23G H 0.4884 0.2335 0.5654 0.042 Uiso 0.5 calc A 1
H23H H 0.3721 0.2274 0.5809 0.042 Uiso 0.5 calc A 1
N261 N 0.4991(5) 0.3054(5) 0.6570(4) 0.0349(15) Uani 0.5 d A 2
C262 C 0.5245(10) 0.2488(8) 0.5910(7) 0.018(2) Uani 0.5 d A 2
H26A H 0.4654 0.2413 0.5337 0.022 Uiso 0.5 calc A 2
H26B H 0.5986 0.2779 0.5878 0.022 Uiso 0.5 calc A 2
C263 C 0.5275(11) 0.1644(8) 0.6145(8) 0.022(3) Uani 0.5 d A 2
H26C H 0.4503 0.1305 0.6078 0.027 Uiso 0.5 calc A 2
H26D H 0.5548 0.1344 0.5769 0.027 Uiso 0.5 calc A 2
O264 O 0.6029(5) 0.1767(4) 0.7021(4) 0.0461(14) Uani 0.5 d A 2
C265 C 0.5822(15) 0.2172(11) 0.7577(9) 0.030(3) Uani 0.5 d A 2
H26E H 0.6407 0.2218 0.8146 0.036 Uiso 0.5 calc A 2
H26F H 0.5075 0.1869 0.7591 0.036 Uiso 0.5 calc A 2
C266 C 0.5810(12) 0.3047(9) 0.7381(8) 0.024(3) Uani 0.5 d A 2
H26G H 0.5655 0.3352 0.7831 0.028 Uiso 0.5 calc A 2
H26H H 0.6573 0.3355 0.7401 0.028 Uiso 0.5 calc A 2
C23 C 0.2876(5) 0.3055(4) 0.7099(4) 0.0205(13) Uani 1 d . .
H23I H 0.2738 0.3489 0.7446 0.025 Uiso 1 calc . .
H23J H 0.3621 0.2972 0.7418 0.025 Uiso 1 calc . .
C24 C 0.1938(5) 0.2250(4) 0.6857(4) 0.0206(13) Uani 1 d . .
H24A H 0.2235 0.1759 0.6863 0.025 Uiso 1 calc . .
H24B H 0.151 0.2219 0.7244 0.025 Uiso 1 calc . .
N25 N 0.1225(4) 0.2298(3) 0.5982(3) 0.0159(10) Uani 1 d . .
C251 C 0.0114(5) 0.1737(4) 0.5570(4) 0.0178(12) Uani 1 d . .
C252 C -0.0714(5) 0.1756(4) 0.5904(4) 0.0173(12) Uani 1 d . .
C253 C -0.1839(5) 0.1219(4) 0.5463(4) 0.0250(14) Uani 1 d . .
H253 H -0.2413 0.1234 0.5686 0.03 Uiso 1 calc . .
C254 C -0.2104(5) 0.0688(4) 0.4730(4) 0.0238(14) Uani 1 d . .
H254 H -0.2865 0.0349 0.444 0.029 Uiso 1 calc . .
C255 C -0.1560(6) 0.0034(4) 0.3638(4) 0.0223(13) Uani 1 d . .
H255 H -0.2315 -0.0316 0.3351 0.027 Uiso 1 calc . .
C256 C -0.0706(6) -0.0014(4) 0.3342(4) 0.0297(15) Uani 1 d . .
H256 H -0.0889 -0.0376 0.2823 0.036 Uiso 1 calc . .
C257 C 0.0433(6) 0.0464(4) 0.3793(4) 0.0260(14) Uani 1 d . .
H257 H 0.1007 0.0397 0.359 0.031 Uiso 1 calc . .
C258 C 0.0721(5) 0.1025(4) 0.4524(4) 0.0200(13) Uani 1 d . .
H258 H 0.1492 0.1337 0.4824 0.024 Uiso 1 calc . .
C259 C -0.1268(5) 0.0630(4) 0.4393(4) 0.0208(13) Uani 1 d . .
C250 C -0.0128(5) 0.1140(4) 0.4830(4) 0.0176(12) Uani 1 d . .
N241 N -0.0454(4) 0.2319(3) 0.6666(3) 0.0188(11) Uani 1 d . .
C242 C -0.0343(6) 0.3195(4) 0.6570(5) 0.0298(15) Uani 1 d . .
H24C H -0.1097 0.3265 0.6257 0.036 Uiso 1 calc . .
H24D H 0.0154 0.3373 0.6244 0.036 Uiso 1 calc . .
C243 C 0.0167(7) 0.3720(4) 0.7454(5) 0.0336(16) Uani 1 d . .
H24E H 0.0933 0.3662 0.7752 0.04 Uiso 1 calc . .
H24F H 0.0249 0.4317 0.7403 0.04 Uiso 1 calc . .
O244 O -0.0524(5) 0.3469(3) 0.7942(4) 0.0401(13) Uani 1 d . .
C245 C -0.0608(8) 0.2621(5) 0.8034(5) 0.040(2) Uani 1 d . .
H24G H -0.1067 0.2447 0.8388 0.048 Uiso 1 calc . .
H24H H 0.016 0.2565 0.833 0.048 Uiso 1 calc . .
C246 C -0.1153(7) 0.2052(5) 0.7172(5) 0.0344(17) Uani 1 d . .
H24I H -0.1202 0.1463 0.7246 0.041 Uiso 1 calc . .
H24J H -0.193 0.209 0.6878 0.041 Uiso 1 calc . .



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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C11 2.072(6) . ?
Ir1 C112 2.102(6) . ?
Ir1 C111 2.135(6) . ?
Ir1 C116 2.165(6) . ?
Ir1 C115 2.205(6) . ?
Ir1 Cl1 2.3713(15) . ?
Ir2 C21 2.055(6) . ?
Ir2 C216 2.100(6) . ?
Ir2 C215 2.125(6) . ?
Ir2 C212 2.169(6) . ?
Ir2 C211 2.195(6) . ?
Ir2 Cl2 2.3685(15) . ?
C111 C112 1.429(9) . ?
C111 C118 1.529(9) . ?
C111 H111 0.95 . ?
C112 C113 1.518(9) . ?
C112 H112 0.95 . ?
C113 C114 1.515(9) . ?
C113 H11A 0.99 . ?
C113 H11B 0.99 . ?
C114 C115 1.510(9) . ?
C114 H11C 0.99 . ?
C114 H11D 0.99 . ?
C115 C116 1.387(10) . ?
C115 H115 0.95 . ?
C116 C117 1.514(10) . ?
C116 H116 0.95 . ?
C117 C118 1.537(10) . ?
C117 H11E 0.99 . ?
C117 H11F 0.99 . ?
C118 H11G 0.99 . ?
C118 H11H 0.99 . ?
C11 N15 1.342(8) . ?
C11 N12 1.361(8) . ?
N12 C121 1.435(7) . ?
N12 C13 1.484(8) . ?
C121 C122 1.382(9) . ?
C121 C120 1.436(9) . ?
C122 C123 1.417(9) . ?
C122 N131 1.434(8) . ?
C123 C124 1.356(10) . ?
C123 H123 0.95 . ?
C124 C129 1.422(9) . ?
C124 H124 0.95 . ?
C125 C126 1.412(10) . ?
C125 C129 1.442(9) . ?
C125 H125 0.95 . ?
C126 C127 1.413(10) . ?
C126 H126 0.95 . ?
C127 C128 1.358(9) . ?
C127 H127 0.95 . ?
C128 C120 1.422(9) . ?
C128 H128 0.95 . ?
C129 C120 1.404(9) . ?
N131 C136 1.457(8) . ?
N131 C132 1.469(9) . ?
C132 C133 1.506(11) . ?
C132 H13A 0.99 . ?
C132 H13B 0.99 . ?
C133 O134 1.409(9) . ?
C133 H13C 0.99 . ?
C133 H13D 0.99 . ?
O134 C135 1.431(9) . ?
C135 C136 1.512(10) . ?
C135 H13E 0.99 . ?
C135 H13F 0.99 . ?
C136 H13G 0.99 . ?
C136 H13H 0.99 . ?
C13 C14 1.507(9) . ?
C13 H13I 0.99 . ?
C13 H13J 0.99 . ?
C14 N15 1.479(8) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
N15 C151 1.435(8) . ?
C151 C152 1.396(9) . ?
C151 C150 1.426(10) . ?
C152 N141 1.410(9) . ?
C152 C153 1.417(9) . ?
C153 C154 1.358(11) . ?
C153 H153 0.95 . ?
C154 C159 1.394(10) . ?
C154 H154 0.95 . ?
C155 C156 1.364(11) . ?
C155 C159 1.409(10) . ?
C155 H155 0.95 . ?
C156 C157 1.403(10) . ?
C156 H156 0.95 . ?
C157 C158 1.380(10) . ?
C157 H157 0.95 . ?
C158 C150 1.416(9) . ?
C158 H158 0.95 . ?
C159 C150 1.422(9) . ?
N141 C142 1.457(8) . ?
N141 C146 1.476(9) . ?
C142 C143 1.511(10) . ?
C142 H14C 0.99 . ?
C142 H14D 0.99 . ?
C143 O144 1.426(9) . ?
C143 H14E 0.99 . ?
C143 H14F 0.99 . ?
O144 C145 1.426(10) . ?
C145 C146 1.504(13) . ?
C145 H14G 0.99 . ?
C145 H14H 0.99 . ?
C146 H14I 0.99 . ?
C146 H14J 0.99 . ?
C211 C212 1.387(10) . ?
C211 C218 1.517(9) . ?
C211 H211 0.95 . ?
C212 C213 1.501(10) . ?
C212 H212 0.95 . ?
C213 C214 1.544(10) . ?
C213 H21A 0.99 . ?
C213 H21B 0.99 . ?
C214 C215 1.540(9) . ?
C214 H21C 0.99 . ?
C214 H21D 0.99 . ?
C215 C216 1.412(9) . ?
C215 H215 0.95 . ?
C216 C217 1.521(9) . ?
C216 H216 0.95 . ?
C217 C218 1.530(9) . ?
C217 H21E 0.99 . ?
C217 H21F 0.99 . ?
C218 H21G 0.99 . ?
C218 H21H 0.99 . ?
C21 N22 1.347(8) . ?
C21 N25 1.367(8) . ?
N22 C221 1.425(8) . ?
N22 C23 1.480(8) . ?
C221 C222 1.372(10) . ?
C221 C220 1.437(10) . ?
C222 C223 1.431(10) . ?
C222 N261 1.438(10) . ?
C222 N231 1.438(10) . ?
C223 C224 1.345(12) . ?
C223 H223 0.95 . ?
C224 C229 1.400(12) . ?
C224 H224 0.95 . ?
C225 C226 1.361(13) . ?
C225 C229 1.413(12) . ?
C225 H225 0.95 . ?
C226 C227 1.411(11) . ?
C226 H226 0.95 . ?
C227 C228 1.372(11) . ?
C227 H227 0.95 . ?
C228 C220 1.420(10) . ?
C228 H228 0.95 . ?
C229 C220 1.426(9) . ?
N231 C236 1.238(16) . ?
N231 C232 1.524(17) . ?
C232 C233 1.49(3) . ?
C232 H23A 0.99 . ?
C232 H23B 0.99 . ?
C233 O234 1.56(2) . ?
C233 H23C 0.99 . ?
C233 H23D 0.99 . ?
O234 C235 1.533(16) . ?
C235 C236 1.52(2) . ?
C235 H23E 0.99 . ?
C235 H23F 0.99 . ?
C236 H23G 0.99 . ?
C236 H23H 0.99 . ?
N261 C266 1.428(14) . ?
N261 C262 1.582(13) . ?
C262 C263 1.499(18) . ?
C262 H26A 0.99 . ?
C262 H26B 0.99 . ?
C263 O264 1.441(13) . ?
C263 H26C 0.99 . ?
C263 H26D 0.99 . ?
O264 C265 1.260(16) . ?
C265 C266 1.53(2) . ?
C265 H26E 0.99 . ?
C265 H26F 0.99 . ?
C266 H26G 0.99 . ?
C266 H26H 0.99 . ?
C23 C24 1.498(9) . ?
C23 H23I 0.99 . ?
C23 H23J 0.99 . ?
C24 N25 1.479(8) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
N25 C251 1.422(8) . ?
C251 C252 1.384(9) . ?
C251 C250 1.434(8) . ?
C252 N241 1.426(8) . ?
C252 C253 1.426(8) . ?
C253 C254 1.357(9) . ?
C253 H253 0.95 . ?
C254 C259 1.412(9) . ?
C254 H254 0.95 . ?
C255 C256 1.384(10) . ?
C255 C259 1.438(9) . ?
C255 H255 0.95 . ?
C256 C257 1.412(10) . ?
C256 H256 0.95 . ?
C257 C258 1.375(9) . ?
C257 H257 0.95 . ?
C258 C250 1.419(9) . ?
C258 H258 0.95 . ?
C259 C250 1.425(9) . ?
N241 C242 1.460(8) . ?
N241 C246 1.463(8) . ?
C242 C243 1.515(10) . ?
C242 H24C 0.99 . ?
C242 H24D 0.99 . ?
C243 O244 1.426(9) . ?
C243 H24E 0.99 . ?
C243 H24F 0.99 . ?
O244 C245 1.418(10) . ?
C245 C246 1.516(10) . ?
C245 H24G 0.99 . ?
C245 H24H 0.99 . ?
C246 H24I 0.99 . ?
C246 H24J 0.99 . ?

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
C11 Ir1 C112 97.2(2) . . ?
C11 Ir1 C111 96.7(2) . . ?
C112 Ir1 C111 39.4(2) . . ?
C11 Ir1 C116 153.3(2) . . ?
C112 Ir1 C116 97.3(2) . . ?
C111 Ir1 C116 80.8(2) . . ?
C11 Ir1 C115 169.3(2) . . ?
C112 Ir1 C115 80.2(2) . . ?
C111 Ir1 C115 87.8(2) . . ?
C116 Ir1 C115 37.0(3) . . ?
C11 Ir1 Cl1 90.73(15) . . ?
C112 Ir1 Cl1 150.84(18) . . ?
C111 Ir1 Cl1 166.29(18) . . ?
C116 Ir1 Cl1 87.45(18) . . ?
C115 Ir1 Cl1 86.93(17) . . ?
C21 Ir2 C216 95.7(2) . . ?
C21 Ir2 C215 96.3(2) . . ?
C216 Ir2 C215 39.1(3) . . ?
C21 Ir2 C212 155.2(3) . . ?
C216 Ir2 C212 97.2(2) . . ?
C215 Ir2 C212 80.8(2) . . ?
C21 Ir2 C211 167.5(3) . . ?
C216 Ir2 C211 80.7(2) . . ?
C215 Ir2 C211 88.5(2) . . ?
C212 Ir2 C211 37.1(3) . . ?
C21 Ir2 Cl2 90.54(17) . . ?
C216 Ir2 Cl2 154.74(18) . . ?
C215 Ir2 Cl2 163.75(18) . . ?
C212 Ir2 Cl2 86.79(18) . . ?
C211 Ir2 Cl2 87.89(18) . . ?
C112 C111 C118 125.5(6) . . ?
C112 C111 Ir1 69.1(3) . . ?
C118 C111 Ir1 114.0(4) . . ?
C112 C111 H111 117.2 . . ?
C118 C111 H111 117.2 . . ?
Ir1 C111 H111 86.9 . . ?
C111 C112 C113 126.7(6) . . ?
C111 C112 Ir1 71.5(3) . . ?
C113 C112 Ir1 110.0(4) . . ?
C111 C112 H112 116.6 . . ?
C113 C112 H112 116.6 . . ?
Ir1 C112 H112 88.3 . . ?
C114 C113 C112 112.5(5) . . ?
C114 C113 H11A 109.1 . . ?
C112 C113 H11A 109.1 . . ?
C114 C113 H11B 109.1 . . ?
C112 C113 H11B 109.1 . . ?
H11A C113 H11B 107.8 . . ?
C115 C114 C113 110.3(5) . . ?
C115 C114 H11C 109.6 . . ?
C113 C114 H11C 109.6 . . ?
C115 C114 H11D 109.6 . . ?
C113 C114 H11D 109.6 . . ?
H11C C114 H11D 108.1 . . ?
C116 C115 C114 125.7(6) . . ?
C116 C115 Ir1 69.9(4) . . ?
C114 C115 Ir1 112.6(4) . . ?
C116 C115 H115 117.2 . . ?
C114 C115 H115 117.2 . . ?
Ir1 C115 H115 87.4 . . ?
C115 C116 C117 126.2(6) . . ?
C115 C116 Ir1 73.1(4) . . ?
C117 C116 Ir1 109.7(4) . . ?
C115 C116 H116 116.9 . . ?
C117 C116 H116 116.9 . . ?
Ir1 C116 H116 87.1 . . ?
C116 C117 C118 112.1(6) . . ?
C116 C117 H11E 109.2 . . ?
C118 C117 H11E 109.2 . . ?
C116 C117 H11F 109.2 . . ?
C118 C117 H11F 109.2 . . ?
H11E C117 H11F 107.9 . . ?
C111 C118 C117 111.7(6) . . ?
C111 C118 H11G 109.3 . . ?
C117 C118 H11G 109.3 . . ?
C111 C118 H11H 109.3 . . ?
C117 C118 H11H 109.3 . . ?
H11G C118 H11H 107.9 . . ?
N15 C11 N12 106.4(5) . . ?
N15 C11 Ir1 123.8(4) . . ?
N12 C11 Ir1 129.7(4) . . ?
C11 N12 C121 127.8(5) . . ?
C11 N12 C13 112.3(5) . . ?
C121 N12 C13 119.1(5) . . ?
C122 C121 N12 119.3(5) . . ?
C122 C121 C120 120.6(5) . . ?
N12 C121 C120 120.1(5) . . ?
C121 C122 C123 119.3(6) . . ?
C121 C122 N131 120.1(5) . . ?
C123 C122 N131 120.6(6) . . ?
C124 C123 C122 121.2(6) . . ?
C124 C123 H123 119.4 . . ?
C122 C123 H123 119.4 . . ?
C123 C124 C129 120.4(6) . . ?
C123 C124 H124 119.8 . . ?
C129 C124 H124 119.8 . . ?
C126 C125 C129 116.3(6) . . ?
C126 C125 H125 121.9 . . ?
C129 C125 H125 121.9 . . ?
C125 C126 C127 121.5(6) . . ?
C125 C126 H126 119.2 . . ?
C127 C126 H126 119.2 . . ?
C128 C127 C126 121.1(6) . . ?
C128 C127 H127 119.5 . . ?
C126 C127 H127 119.5 . . ?
C127 C128 C120 120.3(6) . . ?
C127 C128 H128 119.9 . . ?
C120 C128 H128 119.9 . . ?
C120 C129 C124 119.9(6) . . ?
C120 C129 C125 121.6(6) . . ?
C124 C129 C125 118.5(6) . . ?
C129 C120 C128 119.2(6) . . ?
C129 C120 C121 118.3(6) . . ?
C128 C120 C121 122.5(6) . . ?
C122 N131 C136 115.3(5) . . ?
C122 N131 C132 113.2(5) . . ?
C136 N131 C132 108.9(5) . . ?
N131 C132 C133 108.6(7) . . ?
N131 C132 H13A 110 . . ?
C133 C132 H13A 110 . . ?
N131 C132 H13B 110 . . ?
C133 C132 H13B 110 . . ?
H13A C132 H13B 108.4 . . ?
O134 C133 C132 111.9(6) . . ?
O134 C133 H13C 109.2 . . ?
C132 C133 H13C 109.2 . . ?
O134 C133 H13D 109.2 . . ?
C132 C133 H13D 109.2 . . ?
H13C C133 H13D 107.9 . . ?
C133 O134 C135 109.0(6) . . ?
O134 C135 C136 110.3(6) . . ?
O134 C135 H13E 109.6 . . ?
C136 C135 H13E 109.6 . . ?
O134 C135 H13F 109.6 . . ?
C136 C135 H13F 109.6 . . ?
H13E C135 H13F 108.1 . . ?
N131 C136 C135 109.9(6) . . ?
N131 C136 H13G 109.7 . . ?
C135 C136 H13G 109.7 . . ?
N131 C136 H13H 109.7 . . ?
C135 C136 H13H 109.7 . . ?
H13G C136 H13H 108.2 . . ?
N12 C13 C14 101.7(5) . . ?
N12 C13 H13I 111.4 . . ?
C14 C13 H13I 111.4 . . ?
N12 C13 H13J 111.4 . . ?
C14 C13 H13J 111.4 . . ?
H13I C13 H13J 109.3 . . ?
N15 C14 C13 101.4(5) . . ?
N15 C14 H14A 111.5 . . ?
C13 C14 H14A 111.5 . . ?
N15 C14 H14B 111.5 . . ?
C13 C14 H14B 111.5 . . ?
H14A C14 H14B 109.3 . . ?
C11 N15 C151 126.3(5) . . ?
C11 N15 C14 113.4(5) . . ?
C151 N15 C14 119.6(5) . . ?
C152 C151 C150 121.0(6) . . ?
C152 C151 N15 120.8(6) . . ?
C150 C151 N15 117.9(6) . . ?
C151 C152 N141 122.2(6) . . ?
C151 C152 C153 117.0(6) . . ?
N141 C152 C153 120.8(6) . . ?
C154 C153 C152 122.5(6) . . ?
C154 C153 H153 118.8 . . ?
C152 C153 H153 118.8 . . ?
C153 C154 C159 121.5(6) . . ?
C153 C154 H154 119.3 . . ?
C159 C154 H154 119.3 . . ?
C156 C155 C159 121.4(6) . . ?
C156 C155 H155 119.3 . . ?
C159 C155 H155 119.3 . . ?
C155 C156 C157 119.7(7) . . ?
C155 C156 H156 120.2 . . ?
C157 C156 H156 120.2 . . ?
C158 C157 C156 120.8(7) . . ?
C158 C157 H157 119.6 . . ?
C156 C157 H157 119.6 . . ?
C157 C158 C150 120.2(6) . . ?
C157 C158 H158 119.9 . . ?
C150 C158 H158 119.9 . . ?
C154 C159 C155 122.7(6) . . ?
C154 C159 C150 118.2(6) . . ?
C155 C159 C150 119.0(6) . . ?
C158 C150 C159 118.5(6) . . ?
C158 C150 C151 122.2(6) . . ?
C159 C150 C151 119.3(6) . . ?
C152 N141 C142 119.7(5) . . ?
C152 N141 C146 116.8(6) . . ?
C142 N141 C146 108.1(5) . . ?
N141 C142 C143 110.6(6) . . ?
N141 C142 H14C 109.5 . . ?
C143 C142 H14C 109.5 . . ?
N141 C142 H14D 109.5 . . ?
C143 C142 H14D 109.5 . . ?
H14C C142 H14D 108.1 . . ?
O144 C143 C142 112.0(6) . . ?
O144 C143 H14E 109.2 . . ?
C142 C143 H14E 109.2 . . ?
O144 C143 H14F 109.2 . . ?
C142 C143 H14F 109.2 . . ?
H14E C143 H14F 107.9 . . ?
C143 O144 C145 109.3(6) . . ?
O144 C145 C146 112.4(6) . . ?
O144 C145 H14G 109.1 . . ?
C146 C145 H14G 109.1 . . ?
O144 C145 H14H 109.1 . . ?
C146 C145 H14H 109.1 . . ?
H14G C145 H14H 107.9 . . ?
N141 C146 C145 109.4(7) . . ?
N141 C146 H14I 109.8 . . ?
C145 C146 H14I 109.8 . . ?
N141 C146 H14J 109.8 . . ?
C145 C146 H14J 109.8 . . ?
H14I C146 H14J 108.2 . . ?
C212 C211 C218 123.8(6) . . ?
C212 C211 Ir2 70.4(4) . . ?
C218 C211 Ir2 112.4(4) . . ?
C212 C211 H211 118.1 . . ?
C218 C211 H211 118.1 . . ?
Ir2 C211 H211 87.1 . . ?
C211 C212 C213 128.9(6) . . ?
C211 C212 Ir2 72.5(4) . . ?
C213 C212 Ir2 108.8(4) . . ?
C211 C212 H212 115.5 . . ?
C213 C212 H212 115.5 . . ?
Ir2 C212 H212 88.5 . . ?
C212 C213 C214 111.8(6) . . ?
C212 C213 H21A 109.2 . . ?
C214 C213 H21A 109.2 . . ?
C212 C213 H21B 109.2 . . ?
C214 C213 H21B 109.2 . . ?
H21A C213 H21B 107.9 . . ?
C215 C214 C213 110.5(6) . . ?
C215 C214 H21C 109.5 . . ?
C213 C214 H21C 109.5 . . ?
C215 C214 H21D 109.5 . . ?
C213 C214 H21D 109.5 . . ?
H21C C214 H21D 108.1 . . ?
C216 C215 C214 125.4(6) . . ?
C216 C215 Ir2 69.5(3) . . ?
C214 C215 Ir2 114.0(4) . . ?
C216 C215 H215 117.3 . . ?
C214 C215 H215 117.3 . . ?
Ir2 C215 H215 86.4 . . ?
C215 C216 C217 126.1(6) . . ?
C215 C216 Ir2 71.4(4) . . ?
C217 C216 Ir2 111.0(4) . . ?
C215 C216 H216 117 . . ?
C217 C216 H216 117 . . ?
Ir2 C216 H216 87.5 . . ?
C216 C217 C218 112.0(5) . . ?
C216 C217 H21E 109.2 . . ?
C218 C217 H21E 109.2 . . ?
C216 C217 H21F 109.2 . . ?
C218 C217 H21F 109.2 . . ?
H21E C217 H21F 107.9 . . ?
C211 C218 C217 111.1(5) . . ?
C211 C218 H21G 109.4 . . ?
C217 C218 H21G 109.4 . . ?
C211 C218 H21H 109.4 . . ?
C217 C218 H21H 109.4 . . ?
H21G C218 H21H 108 . . ?
N22 C21 N25 107.2(5) . . ?
N22 C21 Ir2 124.3(4) . . ?
N25 C21 Ir2 128.4(4) . . ?
C21 N22 C221 127.3(5) . . ?
C21 N22 C23 112.4(5) . . ?
C221 N22 C23 119.9(5) . . ?
C222 C221 N22 120.3(6) . . ?
C222 C221 C220 120.2(6) . . ?
N22 C221 C220 119.4(6) . . ?
C221 C222 C223 118.6(7) . . ?
C221 C222 N261 121.1(6) . . ?
C223 C222 N261 120.3(6) . . ?
C221 C222 N231 121.1(6) . . ?
C223 C222 N231 120.3(6) . . ?
C224 C223 C222 121.8(7) . . ?
C224 C223 H223 119.1 . . ?
C222 C223 H223 119.1 . . ?
C223 C224 C229 121.2(7) . . ?
C223 C224 H224 119.4 . . ?
C229 C224 H224 119.4 . . ?
C226 C225 C229 121.5(7) . . ?
C226 C225 H225 119.2 . . ?
C229 C225 H225 119.2 . . ?
C225 C226 C227 119.4(8) . . ?
C225 C226 H226 120.3 . . ?
C227 C226 H226 120.3 . . ?
C228 C227 C226 121.0(8) . . ?
C228 C227 H227 119.5 . . ?
C226 C227 H227 119.5 . . ?
C227 C228 C220 120.3(6) . . ?
C227 C228 H228 119.9 . . ?
C220 C228 H228 119.9 . . ?
C224 C229 C225 122.4(7) . . ?
C224 C229 C220 118.7(7) . . ?
C225 C229 C220 118.9(7) . . ?
C228 C220 C229 118.4(7) . . ?
C228 C220 C221 122.6(6) . . ?
C229 C220 C221 119.0(6) . . ?
C236 N231 C222 123.1(9) . . ?
C236 N231 C232 117.8(11) . . ?
C222 N231 C232 104.8(9) . . ?
C233 C232 N231 103.2(15) . . ?
C233 C232 H23A 111.1 . . ?
N231 C232 H23A 111.1 . . ?
C233 C232 H23B 111.1 . . ?
N231 C232 H23B 111.1 . . ?
H23A C232 H23B 109.1 . . ?
C232 C233 O234 110.9(12) . . ?
C232 C233 H23C 109.5 . . ?
O234 C233 H23C 109.5 . . ?
C232 C233 H23D 109.5 . . ?
O234 C233 H23D 109.5 . . ?
H23C C233 H23D 108.1 . . ?
C235 O234 C233 96.8(10) . . ?
C236 C235 O234 111.3(12) . . ?
C236 C235 H23E 109.4 . . ?
O234 C235 H23E 109.4 . . ?
C236 C235 H23F 109.4 . . ?
O234 C235 H23F 109.4 . . ?
H23E C235 H23F 108 . . ?
N231 C236 C235 107.1(13) . . ?
N231 C236 H23G 110.3 . . ?
C235 C236 H23G 110.3 . . ?
N231 C236 H23H 110.3 . . ?
C235 C236 H23H 110.3 . . ?
H23G C236 H23H 108.6 . . ?
C266 N261 C222 122.3(8) . . ?
C266 N261 C262 104.6(8) . . ?
C222 N261 C262 116.1(6) . . ?
C263 C262 N261 112.6(9) . . ?
C263 C262 H26A 109.1 . . ?
N261 C262 H26A 109.1 . . ?
C263 C262 H26B 109.1 . . ?
N261 C262 H26B 109.1 . . ?
H26A C262 H26B 107.8 . . ?
O264 C263 C262 108.2(9) . . ?
O264 C263 H26C 110.1 . . ?
C262 C263 H26C 110.1 . . ?
O264 C263 H26D 110.1 . . ?
C262 C263 H26D 110.1 . . ?
H26C C263 H26D 108.4 . . ?
C265 O264 C263 117.7(10) . . ?
O264 C265 C266 110.6(12) . . ?
O264 C265 H26E 109.5 . . ?
C266 C265 H26E 109.5 . . ?
O264 C265 H26F 109.5 . . ?
C266 C265 H26F 109.5 . . ?
H26E C265 H26F 108.1 . . ?
N261 C266 C265 114.1(11) . . ?
N261 C266 H26G 108.7 . . ?
C265 C266 H26G 108.7 . . ?
N261 C266 H26H 108.7 . . ?
C265 C266 H26H 108.7 . . ?
H26G C266 H26H 107.6 . . ?
N22 C23 C24 101.8(5) . . ?
N22 C23 H23I 111.4 . . ?
C24 C23 H23I 111.4 . . ?
N22 C23 H23J 111.4 . . ?
C24 C23 H23J 111.4 . . ?
H23I C23 H23J 109.3 . . ?
N25 C24 C23 102.4(5) . . ?
N25 C24 H24A 111.3 . . ?
C23 C24 H24A 111.3 . . ?
N25 C24 H24B 111.3 . . ?
C23 C24 H24B 111.3 . . ?
H24A C24 H24B 109.2 . . ?
C21 N25 C251 127.3(5) . . ?
C21 N25 C24 111.4(5) . . ?
C251 N25 C24 121.0(5) . . ?
C252 C251 N25 119.5(5) . . ?
C252 C251 C250 120.6(5) . . ?
N25 C251 C250 119.9(5) . . ?
C251 C252 N241 120.4(5) . . ?
C251 C252 C253 119.1(5) . . ?
N241 C252 C253 120.5(5) . . ?
C254 C253 C252 121.2(6) . . ?
C254 C253 H253 119.4 . . ?
C252 C253 H253 119.4 . . ?
C253 C254 C259 121.0(6) . . ?
C253 C254 H254 119.5 . . ?
C259 C254 H254 119.5 . . ?
C256 C255 C259 117.9(6) . . ?
C256 C255 H255 121.1 . . ?
C259 C255 H255 121.1 . . ?
C255 C256 C257 121.5(6) . . ?
C255 C256 H256 119.3 . . ?
C257 C256 H256 119.3 . . ?
C258 C257 C256 120.9(6) . . ?
C258 C257 H257 119.6 . . ?
C256 C257 H257 119.6 . . ?
C257 C258 C250 120.3(6) . . ?
C257 C258 H258 119.9 . . ?
C250 C258 H258 119.9 . . ?
C254 C259 C250 119.2(6) . . ?
C254 C259 C255 119.9(6) . . ?
C250 C259 C255 120.8(6) . . ?
C258 C250 C259 118.6(5) . . ?
C258 C250 C251 122.8(5) . . ?
C259 C250 C251 118.6(6) . . ?
C252 N241 C242 115.5(5) . . ?
C252 N241 C246 115.5(5) . . ?
C242 N241 C246 110.9(5) . . ?
N241 C242 C243 108.0(6) . . ?
N241 C242 H24C 110.1 . . ?
C243 C242 H24C 110.1 . . ?
N241 C242 H24D 110.1 . . ?
C243 C242 H24D 110.1 . . ?
H24C C242 H24D 108.4 . . ?
O244 C243 C242 111.4(6) . . ?
O244 C243 H24E 109.4 . . ?
C242 C243 H24E 109.4 . . ?
O244 C243 H24F 109.4 . . ?
C242 C243 H24F 109.4 . . ?
H24E C243 H24F 108 . . ?
C245 O244 C243 109.0(5) . . ?
O244 C245 C246 111.0(7) . . ?
O244 C245 H24G 109.4 . . ?
C246 C245 H24G 109.4 . . ?
O244 C245 H24H 109.4 . . ?
C246 C245 H24H 109.4 . . ?
H24G C245 H24H 108 . . ?
N241 C246 C245 108.2(6) . . ?
N241 C246 H24I 110.1 . . ?
C245 C246 H24I 110.1 . . ?
N241 C246 H24J 110.1 . . ?
C245 C246 H24J 110.1 . . ?
H24I C246 H24J 108.4 . . ?

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

data_rda640
_database_code_depnum_ccdc_archive 'CCDC 1518965'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT214_rda640              
;
PROBLEM: Atom O1W     (Anion/Solvent) ADP max/min Ratio          7.4 prolat

RESPONSE: The population of the O1W atom is equal 0.25. Could be result
of unresolved minor disorder.
;

_vrf_PLAT971_rda640              
;
PROBLEM: Check Calcd Residual Density  0.61A From     Ir1       3.90 eA-3 
 
         
RESPONSE: This may be due in part to the disordered apparent throughout 
the structure.
;

#==============================================================================

# 6. CRYSTALLOGRAPHY

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C33 H32 Cl Ir N4 O4, 0.75(C D2 Cl2), 0.25(H2 O)'
_chemical_formula_sum            'C33.75 H32.50 Cl2.50 D1.50 Ir N4 O4.25'
_chemical_formula_weight         845.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.8111(3)
_cell_length_b                   11.5132(3)
_cell_length_c                   15.6027(3)
_cell_angle_alpha                74.248(2)
_cell_angle_beta                 88.409(2)
_cell_angle_gamma                80.650(2)
_cell_volume                     1673.47(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27816
_cell_measurement_theta_min      3.112
_cell_measurement_theta_max      36.943

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             836
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.233
_shelx_estimated_absorpt_T_min   0.303
_shelx_estimated_absorpt_T_max   0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S, Sapphire3 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_reflns_number            60875
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.027
_diffrn_reflns_theta_max         37.265
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             16783
_reflns_number_gt                15305
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²+3.8000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16783
_refine_ls_number_parameters     434
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.46395(2) 0.33551(2) 0.27023(2) 0.01898(3) Uani 1 1 d . . . . .
Cl1 Cl 0.52095(10) 0.52671(10) 0.21664(7) 0.02522(18) Uani 0.75 1 d . . P A 1
C12 C 0.4279(7) 0.1693(6) 0.3136(3) 0.0331(14) Uani 0.75 1 d D . P A 1
O12 O 0.3980(4) 0.0799(3) 0.3452(3) 0.0403(7) Uani 0.75 1 d D . P A 1
Cl1' Cl 0.4270(5) 0.1457(5) 0.3290(3) 0.02522(18) Uani 0.25 1 d . . P A 2
C12' C 0.4986(19) 0.5068(15) 0.2304(11) 0.0331(14) Uani 0.25 1 d D . P A 2
O12' O 0.5352(11) 0.6001(9) 0.2006(8) 0.0403(7) Uani 0.25 1 d D . P A 2
C11 C 0.6549(3) 0.2723(3) 0.2703(2) 0.0309(6) Uani 1 1 d . . . . .
O11 O 0.7696(3) 0.2362(3) 0.2703(2) 0.0490(7) Uani 1 1 d . . . . .
C1 C 0.2549(2) 0.40653(18) 0.26692(13) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.18481(19) 0.45677(19) 0.32651(12) 0.0168(3) Uani 1 1 d . . . . .
C3 C 0.0348(3) 0.4855(3) 0.30706(16) 0.0262(5) Uani 1 1 d . . . . .
H3A H -0.0036 0.5688 0.3110 0.031 Uiso 1 1 calc R U . . .
H3B H -0.0153 0.4257 0.3481 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0277(3) 0.4760(3) 0.21179(17) 0.0264(5) Uani 1 1 d . . . . .
H4A H -0.0453 0.4293 0.2043 0.032 Uiso 1 1 calc R U . . .
H4B H 0.0111 0.5578 0.1686 0.032 Uiso 1 1 calc R U . . .
N5 N 0.1665(2) 0.40982(18) 0.20203(12) 0.0161(3) Uani 1 1 d . . . . .
C21 C 0.2370(2) 0.4692(2) 0.40735(14) 0.0158(3) Uani 1 1 d . . . . .
C22 C 0.2245(2) 0.3823(2) 0.48664(14) 0.0170(3) Uani 1 1 d . . . . .
C23 C 0.2694(3) 0.4009(2) 0.56717(15) 0.0198(4) Uani 1 1 d . . . . .
H23 H 0.2613 0.3414 0.6219 0.024 Uiso 1 1 calc R U . . .
C24 C 0.3239(3) 0.5025(2) 0.56706(15) 0.0208(4) Uani 1 1 d . . . . .
H24 H 0.3544 0.5122 0.6216 0.025 Uiso 1 1 calc R U . . .
C24A C 0.3358(2) 0.5937(2) 0.48692(16) 0.0189(4) Uani 1 1 d . . . . .
C25 C 0.3920(3) 0.7002(2) 0.48585(19) 0.0243(4) Uani 1 1 d . . . . .
H25 H 0.4236 0.7106 0.5399 0.029 Uiso 1 1 calc R U . . .
C26 C 0.4011(3) 0.7881(3) 0.4075(2) 0.0269(5) Uani 1 1 d . . . . .
H26 H 0.4391 0.8590 0.4074 0.032 Uiso 1 1 calc R U . . .
C27 C 0.3542(3) 0.7735(3) 0.3271(2) 0.0264(5) Uani 1 1 d . . . . .
H27 H 0.3609 0.8349 0.2731 0.032 Uiso 1 1 calc R U . . .
C28 C 0.2991(3) 0.6723(2) 0.32551(16) 0.0204(4) Uani 1 1 d . . . . .
H28 H 0.2668 0.6647 0.2708 0.025 Uiso 1 1 calc R U . . .
C28A C 0.2901(2) 0.5782(2) 0.40542(14) 0.0170(3) Uani 1 1 d . . . . .
C51 C 0.2032(2) 0.3684(2) 0.12495(14) 0.0166(3) Uani 1 1 d . . . . .
C52 C 0.2366(2) 0.4491(2) 0.04698(14) 0.0166(3) Uani 1 1 d . . . . .
C53 C 0.2732(2) 0.4042(2) -0.02838(15) 0.0204(4) Uani 1 1 d . . . . .
H53 H 0.2946 0.4592 -0.0826 0.024 Uiso 1 1 calc R U . . .
C54 C 0.2782(3) 0.2835(3) -0.02422(17) 0.0229(4) Uani 1 1 d . . . . .
H54 H 0.3078 0.2550 -0.0745 0.027 Uiso 1 1 calc R U . . .
C54A C 0.2400(2) 0.2002(2) 0.05401(17) 0.0211(4) Uani 1 1 d . . . . .
C55 C 0.2389(3) 0.0754(3) 0.0591(2) 0.0282(5) Uani 1 1 d . . . . .
H55 H 0.2715 0.0442 0.0105 0.034 Uiso 1 1 calc R U . . .
C56 C 0.1917(3) -0.0003(3) 0.1331(2) 0.0322(6) Uani 1 1 d . . . . .
H56 H 0.1907 -0.0835 0.1355 0.039 Uiso 1 1 calc R U . . .
C57 C 0.1443(3) 0.0444(3) 0.2061(2) 0.0306(6) Uani 1 1 d . . . . .
H57 H 0.1094 -0.0085 0.2567 0.037 Uiso 1 1 calc R U . . .
C58 C 0.1480(3) 0.1634(2) 0.20492(18) 0.0248(5) Uani 1 1 d . . . . .
H58 H 0.1175 0.1918 0.2551 0.030 Uiso 1 1 calc R U . . .
C58A C 0.1970(2) 0.2440(2) 0.12944(16) 0.0189(4) Uani 1 1 d . . . . .
N221 N 0.1649(2) 0.27653(19) 0.48714(13) 0.0185(3) Uani 1 1 d . . . . .
C222 C 0.0345(3) 0.2744(2) 0.53652(17) 0.0223(4) Uani 1 1 d . . . . .
H22A H -0.0322 0.3489 0.5091 0.027 Uiso 1 1 calc R U . . .
H22B H 0.0519 0.2733 0.5990 0.027 Uiso 1 1 calc R U . . .
C223 C -0.0255(3) 0.1619(3) 0.53461(19) 0.0264(5) Uani 1 1 d . . . . .
H22C H -0.1130 0.1606 0.5679 0.032 Uiso 1 1 calc R U . . .
H22D H -0.0466 0.1652 0.4722 0.032 Uiso 1 1 calc R U . . .
O224 O 0.0690(2) 0.05296(19) 0.57338(14) 0.0283(4) Uani 1 1 d . . . . .
C225 C 0.1932(3) 0.0536(2) 0.5233(2) 0.0272(5) Uani 1 1 d . . . . .
H22E H 0.1717 0.0577 0.4609 0.033 Uiso 1 1 calc R U . . .
H22F H 0.2578 -0.0231 0.5485 0.033 Uiso 1 1 calc R U . . .
C226 C 0.2608(3) 0.1621(2) 0.52565(18) 0.0231(4) Uani 1 1 d . . . . .
H22G H 0.2848 0.1571 0.5879 0.028 Uiso 1 1 calc R U . . .
H22H H 0.3470 0.1612 0.4912 0.028 Uiso 1 1 calc R U . . .
N521 N 0.2322(2) 0.57540(19) 0.04282(13) 0.0169(3) Uani 1 1 d . . . . .
C522 C 0.3592(2) 0.6228(2) 0.00893(17) 0.0204(4) Uani 1 1 d . . . . .
H52A H 0.3715 0.6221 -0.0541 0.025 Uiso 1 1 calc R U . . .
H52B H 0.4401 0.5705 0.0438 0.025 Uiso 1 1 calc R U . . .
C523 C 0.3484(3) 0.7523(2) 0.0167(2) 0.0248(5) Uani 1 1 d . . . . .
H52C H 0.3403 0.7517 0.0802 0.030 Uiso 1 1 calc R U . . .
H52D H 0.4336 0.7849 -0.0061 0.030 Uiso 1 1 calc R U . . .
O524 O 0.2318(2) 0.83003(18) -0.03208(14) 0.0270(4) Uani 1 1 d . . . . .
C525 C 0.1081(3) 0.7827(3) -0.0029(2) 0.0258(5) Uani 1 1 d . . . . .
H52E H 0.0289 0.8364 -0.0389 0.031 Uiso 1 1 calc R U . . .
H52F H 0.0925 0.7826 0.0600 0.031 Uiso 1 1 calc R U . . .
C526 C 0.1145(2) 0.6542(2) -0.01134(17) 0.0218(4) Uani 1 1 d . . . . .
H52G H 0.0276 0.6235 0.0098 0.026 Uiso 1 1 calc R U . . .
H52H H 0.1264 0.6537 -0.0745 0.026 Uiso 1 1 calc R U . . .
C20 C 0.1989(4) 0.0423(3) 0.7875(2) 0.0285(7) Uani 0.75 1 d . . P B 1
H20A D 0.1756 -0.0259 0.8368 0.034 Uiso 0.75 1 calc R U P B 1
H20B D 0.1729 0.0280 0.7308 0.034 Uiso 0.75 1 calc R U P B 1
Cl3 Cl 0.37399(15) 0.04268(19) 0.78960(12) 0.0620(4) Uani 0.75 1 d . . P B 1
Cl4 Cl 0.10304(13) 0.17982(9) 0.79781(6) 0.0355(2) Uani 0.75 1 d . . P B 1
O1W O 0.4261(10) 0.0324(7) 0.8432(6) 0.032(2) Uani 0.25 1 d . . P C 2


_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 C11 1.897(3) . ?
Ir1 C12 1.936(6) . ?
Ir1 C12' 1.983(14) . ?
Ir1 C1 2.077(2) . ?
Ir1 Cl1' 2.214(5) . ?
Ir1 Cl1 2.2874(11) . ?
C12 O12 1.097(6) . ?
C12' O12' 1.159(9) . ?
C11 O11 1.134(4) . ?
C1 N5 1.341(3) . ?
C1 N2 1.342(3) . ?
N2 C21 1.425(3) . ?
N2 C3 1.476(3) . ?
C3 C4 1.524(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N5 1.474(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N5 C51 1.426(3) . ?
C21 C22 1.380(3) . ?
C21 C28A 1.427(3) . ?
C22 C23 1.423(3) . ?
C22 N221 1.432(3) . ?
C23 C24 1.363(4) . ?
C23 H23 0.9500 . ?
C24 C24A 1.414(3) . ?
C24 H24 0.9500 . ?
C24A C25 1.420(4) . ?
C24A C28A 1.425(3) . ?
C25 C26 1.371(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.410(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.367(4) . ?
C27 H27 0.9500 . ?
C28 C28A 1.424(3) . ?
C28 H28 0.9500 . ?
C51 C52 1.383(3) . ?
C51 C58A 1.426(3) . ?
C52 C53 1.423(3) . ?
C52 N521 1.431(3) . ?
C53 C54 1.366(4) . ?
C53 H53 0.9500 . ?
C54 C54A 1.416(4) . ?
C54 H54 0.9500 . ?
C54A C55 1.419(4) . ?
C54A C58A 1.429(3) . ?
C55 C56 1.365(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.411(5) . ?
C56 H56 0.9500 . ?
C57 C58 1.371(4) . ?
C57 H57 0.9500 . ?
C58 C58A 1.414(4) . ?
C58 H58 0.9500 . ?
N221 C222 1.476(3) . ?
N221 C226 1.477(3) . ?
C222 C223 1.515(4) . ?
C222 H22A 0.9900 . ?
C222 H22B 0.9900 . ?
C223 O224 1.428(4) . ?
C223 H22C 0.9900 . ?
C223 H22D 0.9900 . ?
O224 C225 1.429(4) . ?
C225 C226 1.515(4) . ?
C225 H22E 0.9900 . ?
C225 H22F 0.9900 . ?
C226 H22G 0.9900 . ?
C226 H22H 0.9900 . ?
N521 C522 1.469(3) . ?
N521 C526 1.472(3) . ?
C522 C523 1.515(4) . ?
C522 H52A 0.9900 . ?
C522 H52B 0.9900 . ?
C523 O524 1.427(3) . ?
C523 H52C 0.9900 . ?
C523 H52D 0.9900 . ?
O524 C525 1.424(3) . ?
C525 C526 1.511(4) . ?
C525 H52E 0.9900 . ?
C525 H52F 0.9900 . ?
C526 H52G 0.9900 . ?
C526 H52H 0.9900 . ?
C20 Cl3 1.720(5) . ?
C20 Cl4 1.750(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Ir1 C12 88.6(2) . . ?
C11 Ir1 C12' 92.2(6) . . ?
C11 Ir1 C1 178.62(11) . . ?
C12 Ir1 C1 92.1(2) . . ?
C12' Ir1 C1 87.2(6) . . ?
C11 Ir1 Cl1' 87.89(17) . . ?
C12' Ir1 Cl1' 174.1(5) . . ?
C1 Ir1 Cl1' 92.84(15) . . ?
C11 Ir1 Cl1 87.73(11) . . ?
C12 Ir1 Cl1 176.2(2) . . ?
C1 Ir1 Cl1 91.60(6) . . ?
O12 C12 Ir1 171.8(5) . . ?
O12' C12' Ir1 169.9(15) . . ?
O11 C11 Ir1 179.0(3) . . ?
N5 C1 N2 108.16(18) . . ?
N5 C1 Ir1 124.29(15) . . ?
N2 C1 Ir1 127.55(15) . . ?
C1 N2 C21 127.29(18) . . ?
C1 N2 C3 112.26(18) . . ?
C21 N2 C3 119.95(18) . . ?
N2 C3 C4 102.24(18) . . ?
N2 C3 H3A 111.3 . . ?
C4 C3 H3A 111.3 . . ?
N2 C3 H3B 111.3 . . ?
C4 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
N5 C4 C3 101.70(18) . . ?
N5 C4 H4A 111.4 . . ?
C3 C4 H4A 111.4 . . ?
N5 C4 H4B 111.4 . . ?
C3 C4 H4B 111.4 . . ?
H4A C4 H4B 109.3 . . ?
C1 N5 C51 124.88(19) . . ?
C1 N5 C4 112.85(18) . . ?
C51 N5 C4 121.84(18) . . ?
C22 C21 N2 120.1(2) . . ?
C22 C21 C28A 121.13(19) . . ?
N2 C21 C28A 118.5(2) . . ?
C21 C22 C23 119.0(2) . . ?
C21 C22 N221 119.98(19) . . ?
C23 C22 N221 121.0(2) . . ?
C24 C23 C22 121.2(2) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C24A 120.9(2) . . ?
C23 C24 H24 119.5 . . ?
C24A C24 H24 119.5 . . ?
C24 C24A C25 121.5(2) . . ?
C24 C24A C28A 119.1(2) . . ?
C25 C24A C28A 119.3(2) . . ?
C26 C25 C24A 120.6(2) . . ?
C26 C25 H25 119.7 . . ?
C24A C25 H25 119.7 . . ?
C25 C26 C27 120.0(2) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 121.1(3) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C28A 120.4(2) . . ?
C27 C28 H28 119.8 . . ?
C28A C28 H28 119.8 . . ?
C28 C28A C24A 118.6(2) . . ?
C28 C28A C21 122.8(2) . . ?
C24A C28A C21 118.6(2) . . ?
C52 C51 C58A 121.4(2) . . ?
C52 C51 N5 120.4(2) . . ?
C58A C51 N5 118.1(2) . . ?
C51 C52 C53 118.7(2) . . ?
C51 C52 N521 120.02(19) . . ?
C53 C52 N521 121.3(2) . . ?
C54 C53 C52 121.2(2) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C53 C54 C54A 120.9(2) . . ?
C53 C54 H54 119.5 . . ?
C54A C54 H54 119.5 . . ?
C54 C54A C55 122.1(2) . . ?
C54 C54A C58A 119.0(2) . . ?
C55 C54A C58A 118.9(3) . . ?
C56 C55 C54A 120.6(3) . . ?
C56 C55 H55 119.7 . . ?
C54A C55 H55 119.7 . . ?
C55 C56 C57 120.3(3) . . ?
C55 C56 H56 119.8 . . ?
C57 C56 H56 119.8 . . ?
C58 C57 C56 120.7(3) . . ?
C58 C57 H57 119.6 . . ?
C56 C57 H57 119.6 . . ?
C57 C58 C58A 120.4(3) . . ?
C57 C58 H58 119.8 . . ?
C58A C58 H58 119.8 . . ?
C58 C58A C51 122.5(2) . . ?
C58 C58A C54A 119.0(2) . . ?
C51 C58A C54A 118.5(2) . . ?
C22 N221 C222 111.41(19) . . ?
C22 N221 C226 111.85(19) . . ?
C222 N221 C226 109.3(2) . . ?
N221 C222 C223 109.6(2) . . ?
N221 C222 H22A 109.7 . . ?
C223 C222 H22A 109.7 . . ?
N221 C222 H22B 109.7 . . ?
C223 C222 H22B 109.7 . . ?
H22A C222 H22B 108.2 . . ?
O224 C223 C222 110.9(2) . . ?
O224 C223 H22C 109.5 . . ?
C222 C223 H22C 109.5 . . ?
O224 C223 H22D 109.5 . . ?
C222 C223 H22D 109.5 . . ?
H22C C223 H22D 108.0 . . ?
C223 O224 C225 109.1(2) . . ?
O224 C225 C226 110.6(2) . . ?
O224 C225 H22E 109.5 . . ?
C226 C225 H22E 109.5 . . ?
O224 C225 H22F 109.5 . . ?
C226 C225 H22F 109.5 . . ?
H22E C225 H22F 108.1 . . ?
N221 C226 C225 109.5(2) . . ?
N221 C226 H22G 109.8 . . ?
C225 C226 H22G 109.8 . . ?
N221 C226 H22H 109.8 . . ?
C225 C226 H22H 109.8 . . ?
H22G C226 H22H 108.2 . . ?
C52 N521 C522 113.68(19) . . ?
C52 N521 C526 112.27(18) . . ?
C522 N521 C526 108.41(19) . . ?
N521 C522 C523 108.9(2) . . ?
N521 C522 H52A 109.9 . . ?
C523 C522 H52A 109.9 . . ?
N521 C522 H52B 109.9 . . ?
C523 C522 H52B 109.9 . . ?
H52A C522 H52B 108.3 . . ?
O524 C523 C522 111.4(2) . . ?
O524 C523 H52C 109.3 . . ?
C522 C523 H52C 109.3 . . ?
O524 C523 H52D 109.3 . . ?
C522 C523 H52D 109.3 . . ?
H52C C523 H52D 108.0 . . ?
C525 O524 C523 110.6(2) . . ?
O524 C525 C526 111.8(2) . . ?
O524 C525 H52E 109.3 . . ?
C526 C525 H52E 109.3 . . ?
O524 C525 H52F 109.3 . . ?
C526 C525 H52F 109.3 . . ?
H52E C525 H52F 107.9 . . ?
N521 C526 C525 108.6(2) . . ?
N521 C526 H52G 110.0 . . ?
C525 C526 H52G 110.0 . . ?
N521 C526 H52H 110.0 . . ?
C525 C526 H52H 110.0 . . ?
H52G C526 H52H 108.4 . . ?
Cl3 C20 Cl4 112.3(2) . . ?
Cl3 C20 H20A 109.2 . . ?
Cl4 C20 H20A 109.2 . . ?
Cl3 C20 H20B 109.2 . . ?
Cl4 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?

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
N5 C1 N2 C21 178.1(2) . . . . ?
Ir1 C1 N2 C21 -2.2(3) . . . . ?
N5 C1 N2 C3 6.3(3) . . . . ?
Ir1 C1 N2 C3 -174.03(18) . . . . ?
C1 N2 C3 C4 -14.5(3) . . . . ?
C21 N2 C3 C4 173.0(2) . . . . ?
N2 C3 C4 N5 15.8(3) . . . . ?
N2 C1 N5 C51 177.8(2) . . . . ?
Ir1 C1 N5 C51 -1.8(3) . . . . ?
N2 C1 N5 C4 5.4(3) . . . . ?
Ir1 C1 N5 C4 -174.28(18) . . . . ?
C3 C4 N5 C1 -13.9(3) . . . . ?
C3 C4 N5 C51 173.4(2) . . . . ?
C1 N2 C21 C22 -94.9(3) . . . . ?
C3 N2 C21 C22 76.3(3) . . . . ?
C1 N2 C21 C28A 90.9(3) . . . . ?
C3 N2 C21 C28A -97.9(3) . . . . ?
N2 C21 C22 C23 -176.0(2) . . . . ?
C28A C21 C22 C23 -1.9(3) . . . . ?
N2 C21 C22 N221 3.0(3) . . . . ?
C28A C21 C22 N221 177.1(2) . . . . ?
C21 C22 C23 C24 0.1(4) . . . . ?
N221 C22 C23 C24 -178.8(2) . . . . ?
C22 C23 C24 C24A 0.9(4) . . . . ?
C23 C24 C24A C25 179.8(2) . . . . ?
C23 C24 C24A C28A -0.1(4) . . . . ?
C24 C24A C25 C26 -179.2(2) . . . . ?
C28A C24A C25 C26 0.7(4) . . . . ?
C24A C25 C26 C27 0.1(4) . . . . ?
C25 C26 C27 C28 0.0(4) . . . . ?
C26 C27 C28 C28A -1.0(4) . . . . ?
C27 C28 C28A C24A 1.8(4) . . . . ?
C27 C28 C28A C21 -178.3(2) . . . . ?
C24 C24A C28A C28 178.3(2) . . . . ?
C25 C24A C28A C28 -1.6(3) . . . . ?
C24 C24A C28A C21 -1.6(3) . . . . ?
C25 C24A C28A C21 178.4(2) . . . . ?
C22 C21 C28A C28 -177.3(2) . . . . ?
N2 C21 C28A C28 -3.1(3) . . . . ?
C22 C21 C28A C24A 2.7(3) . . . . ?
N2 C21 C28A C24A 176.8(2) . . . . ?
C1 N5 C51 C52 -93.0(3) . . . . ?
C4 N5 C51 C52 78.8(3) . . . . ?
C1 N5 C51 C58A 90.4(3) . . . . ?
C4 N5 C51 C58A -97.8(3) . . . . ?
C58A C51 C52 C53 -3.7(3) . . . . ?
N5 C51 C52 C53 179.8(2) . . . . ?
C58A C51 C52 N521 175.5(2) . . . . ?
N5 C51 C52 N521 -1.1(3) . . . . ?
C51 C52 C53 C54 -1.3(3) . . . . ?
N521 C52 C53 C54 179.6(2) . . . . ?
C52 C53 C54 C54A 3.4(4) . . . . ?
C53 C54 C54A C55 177.5(2) . . . . ?
C53 C54 C54A C58A -0.6(4) . . . . ?
C54 C54A C55 C56 -175.1(3) . . . . ?
C58A C54A C55 C56 3.0(4) . . . . ?
C54A C55 C56 C57 -0.6(4) . . . . ?
C55 C56 C57 C58 -1.6(5) . . . . ?
C56 C57 C58 C58A 1.3(4) . . . . ?
C57 C58 C58A C51 -179.9(2) . . . . ?
C57 C58 C58A C54A 1.2(4) . . . . ?
C52 C51 C58A C58 -172.6(2) . . . . ?
N5 C51 C58A C58 4.0(3) . . . . ?
C52 C51 C58A C54A 6.3(3) . . . . ?
N5 C51 C58A C54A -177.1(2) . . . . ?
C54 C54A C58A C58 174.9(2) . . . . ?
C55 C54A C58A C58 -3.3(3) . . . . ?
C54 C54A C58A C51 -4.1(3) . . . . ?
C55 C54A C58A C51 177.7(2) . . . . ?
C21 C22 N221 C222 -115.5(2) . . . . ?
C23 C22 N221 C222 63.4(3) . . . . ?
C21 C22 N221 C226 121.8(2) . . . . ?
C23 C22 N221 C226 -59.2(3) . . . . ?
C22 N221 C222 C223 179.5(2) . . . . ?
C226 N221 C222 C223 -56.4(3) . . . . ?
N221 C222 C223 O224 59.0(3) . . . . ?
C222 C223 O224 C225 -61.0(3) . . . . ?
C223 O224 C225 C226 61.3(3) . . . . ?
C22 N221 C226 C225 -179.3(2) . . . . ?
C222 N221 C226 C225 56.9(3) . . . . ?
O224 C225 C226 N221 -59.8(3) . . . . ?
C51 C52 N521 C522 128.7(2) . . . . ?
C53 C52 N521 C522 -52.2(3) . . . . ?
C51 C52 N521 C526 -107.8(2) . . . . ?
C53 C52 N521 C526 71.3(3) . . . . ?
C52 N521 C522 C523 -174.1(2) . . . . ?
C526 N521 C522 C523 60.3(2) . . . . ?
N521 C522 C523 O524 -58.9(3) . . . . ?
C522 C523 O524 C525 56.7(3) . . . . ?
C523 O524 C525 C526 -57.1(3) . . . . ?
C52 N521 C526 C525 173.3(2) . . . . ?
C522 N521 C526 C525 -60.3(3) . . . . ?
O524 C525 C526 N521 59.2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3A Cl4 0.99 2.95 3.789(3) 142.9 2_566
C53 H53 Cl1 0.95 2.72 3.502(2) 140.5 2_665
C53 H53 O12' 0.95 2.60 3.243(11) 124.9 2_665
C226 H22H Cl1' 0.99 2.67 3.470(5) 137.9 .
C522 H52B Cl1 0.99 2.72 3.466(3) 132.4 .
C525 H52F Cl4 0.99 2.97 3.849(3) 148.9 2_566
C20 H20A O524 0.99 2.27 3.172(4) 150.5 1_546
C20 H20B O224 0.99 2.61 3.572(5) 164.0 .

_refine_diff_density_max         3.573
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.151

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

data_rda641
_database_code_depnum_ccdc_archive 'CCDC 1518966'
_audit_update_record             
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;

#==============================================================================

# 6. CRYSTALLOGRAPHY

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H36 Cl Ir N4 O2'
_chemical_formula_sum            'C35 H36 Cl Ir N4 O2'
_chemical_formula_weight         772.33

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'
Ir Ir -1.4442 7.9887 '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        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   14.3082(2)
_cell_length_b                   14.41450(10)
_cell_length_c                   15.9946(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.255(2)
_cell_angle_gamma                90
_cell_volume                     3094.82(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22566
_cell_measurement_theta_min      3.806
_cell_measurement_theta_max      36.883
_diffrn_orient_matrix_UB_11      -0.0111622000
_diffrn_orient_matrix_UB_12      0.0470572000
_diffrn_orient_matrix_UB_13      0.0054828000
_diffrn_orient_matrix_UB_21      -0.0400063000
_diffrn_orient_matrix_UB_22      -0.0143275000
_diffrn_orient_matrix_UB_23      0.0135305000
_diffrn_orient_matrix_UB_31      0.0326399000
_diffrn_orient_matrix_UB_32      -0.0014115000
_diffrn_orient_matrix_UB_33      0.0449758000

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.225
_exptl_absorpt_coefficient_mu    4.439
_shelx_estimated_absorpt_T_min   0.259
_shelx_estimated_absorpt_T_max   0.435
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_T_max  0.450
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.0991
0 -1 1 0.1697
0 -1 -1 0.1256
-2 1 4 0.1179
2 -1 -4 0.1441
-3 -1 3 0.1262
3 1 -3 0.1272
3 2 1 0.1173
-3 -3 1 0.1355
-1 5 -4 0.1338
-5 2 2 0.1797
-3 -2 -5 0.1903
4 -5 -2 0.1759
5 -2 -2 0.1666
2 5 0 0.1407
-2 -5 2 0.1571
0 -1 0 0.1369
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            53227
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.683
_diffrn_reflns_theta_max         37.627
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7986
_reflns_number_gt                7177
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+6.2500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7986
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.2500 0.20847(2) 0.5000 0.02478(4) Uani 1 2 d S T P . .
Cl1 Cl 0.19883(13) 0.20486(10) 0.34194(17) 0.0343(3) Uani 0.5 1 d . . P . .
O12 O 0.3159(6) 0.1985(4) 0.6962(4) 0.0510(15) Uani 0.5 1 d . . P A 2
C12 C 0.2907(5) 0.2052(4) 0.6192(6) 0.0315(10) Uani 0.5 1 d . . P A 2
O11 O 0.2500 -0.0006(2) 0.5000 0.0516(8) Uani 1 2 d S T P . .
C11 C 0.2500 0.0758(2) 0.5000 0.0321(6) Uani 1 2 d S T P A .
C1 C 0.2500 0.3537(2) 0.5000 0.0343(7) Uani 1 2 d S T P A .
N2 N 0.33027(16) 0.40819(14) 0.53765(19) 0.0389(5) Uani 1 1 d . . . . .
C3 C 0.3068(2) 0.50800(18) 0.5158(3) 0.0598(11) Uani 1 1 d . . . . .
H3A H 0.3312 0.5290 0.4681 0.072 Uiso 1 1 calc R U . . .
H3B H 0.3357 0.5478 0.5689 0.072 Uiso 1 1 calc R U . . .
C21 C 0.43068(17) 0.37829(16) 0.57864(18) 0.0318(4) Uani 1 1 d . . . . .
C22 C 0.48174(17) 0.40233(16) 0.66729(18) 0.0304(4) Uani 1 1 d . . . . .
C23 C 0.58154(16) 0.37141(18) 0.70668(16) 0.0295(4) Uani 1 1 d . . . . .
H23 H 0.6172 0.3859 0.7673 0.035 Uiso 1 1 calc R U . . .
C24 C 0.62755(17) 0.32139(17) 0.65976(16) 0.0281(4) Uani 1 1 d . . . . .
H24 H 0.6933 0.2990 0.6890 0.034 Uiso 1 1 calc R U . . .
C24A C 0.57893(19) 0.30225(16) 0.56814(16) 0.0287(4) Uani 1 1 d . . . . .
C25 C 0.6289(2) 0.2579(2) 0.5170(2) 0.0394(6) Uani 1 1 d . . . . .
H25 H 0.6945 0.2349 0.5454 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5838(3) 0.2480(3) 0.4270(2) 0.0511(8) Uani 1 1 d . . . . .
H26 H 0.6179 0.2178 0.3932 0.061 Uiso 1 1 calc R U . . .
C27 C 0.4877(3) 0.2820(3) 0.3846(2) 0.0531(9) Uani 1 1 d . . . . .
H27 H 0.4581 0.2772 0.3217 0.064 Uiso 1 1 calc R U . . .
C28A C 0.47913(18) 0.33304(16) 0.52637(16) 0.0299(4) Uani 1 1 d . . . . .
C28 C 0.4355(2) 0.3221(2) 0.43214(19) 0.0434(7) Uani 1 1 d . . . . .
H28 H 0.3694 0.3430 0.4021 0.052 Uiso 1 1 calc R U . . .
N221 N 0.43841(16) 0.45957(16) 0.7152(2) 0.0396(5) Uani 1 1 d . . . . .
C222 C 0.3563(2) 0.4206(2) 0.7388(3) 0.0445(7) Uani 1 1 d . . . . .
H22A H 0.3831 0.3778 0.7899 0.053 Uiso 1 1 calc R U . . .
H22B H 0.3115 0.3848 0.6877 0.053 Uiso 1 1 calc R U . . .
C223 C 0.2984(3) 0.4970(2) 0.7628(4) 0.0626(12) Uani 1 1 d . . . . .
H22C H 0.2445 0.4695 0.7804 0.075 Uiso 1 1 calc R U . . .
H22D H 0.2673 0.5369 0.7101 0.075 Uiso 1 1 calc R U . . .
C224 C 0.3651(3) 0.5553(3) 0.8385(4) 0.0693(14) Uani 1 1 d . . . . .
H22E H 0.3897 0.5176 0.8935 0.083 Uiso 1 1 calc R U . . .
H22F H 0.3268 0.6082 0.8496 0.083 Uiso 1 1 calc R U . . .
C225 C 0.4530(3) 0.5913(3) 0.8149(4) 0.0695(14) Uani 1 1 d . . . . .
H22G H 0.4288 0.6352 0.7644 0.083 Uiso 1 1 calc R U . . .
H22H H 0.4994 0.6252 0.8666 0.083 Uiso 1 1 calc R U . . .
C226 C 0.5078(2) 0.5115(3) 0.7899(3) 0.0561(10) Uani 1 1 d . . . . .
H22I H 0.5632 0.5361 0.7727 0.067 Uiso 1 1 calc R U . . .
H22J H 0.5363 0.4698 0.8417 0.067 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C12 1.792(8) . ?
Ir1 C12 1.792(8) 2_556 ?
Ir1 C11 1.912(4) . ?
Ir1 C1 2.094(3) . ?
Ir1 Cl1 2.377(2) . ?
Ir1 Cl1 2.377(2) 2_556 ?
O12 C12 1.161(9) . ?
C12 Cl1 0.586(7) 2_556 ?
O11 C11 1.102(4) . ?
C1 N2 1.349(3) 2_556 ?
C1 N2 1.349(3) . ?
N2 C21 1.424(3) . ?
N2 C3 1.491(3) . ?
C3 C3 1.526(7) 2_556 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C21 C22 1.395(4) . ?
C21 C28A 1.416(4) . ?
C22 N221 1.408(3) . ?
C22 C23 1.418(3) . ?
C23 C24 1.363(3) . ?
C23 H23 0.9500 . ?
C24 C24A 1.415(3) . ?
C24 H24 0.9500 . ?
C24A C25 1.413(4) . ?
C24A C28A 1.422(4) . ?
C25 C26 1.366(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.395(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.364(6) . ?
C27 H27 0.9500 . ?
C28A C28 1.426(4) . ?
C28 H28 0.9500 . ?
N221 C222 1.465(4) . ?
N221 C226 1.467(4) . ?
C222 C223 1.505(4) . ?
C222 H22A 0.9900 . ?
C222 H22B 0.9900 . ?
C223 C224 1.512(6) . ?
C223 H22C 0.9900 . ?
C223 H22D 0.9900 . ?
C224 C225 1.524(5) . ?
C224 H22E 0.9900 . ?
C224 H22F 0.9900 . ?
C225 C226 1.522(5) . ?
C225 H22G 0.9900 . ?
C225 H22H 0.9900 . ?
C226 H22I 0.9900 . ?
C226 H22J 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Ir1 C12 177.0(3) . 2_556 ?
C12 Ir1 C11 88.49(17) . . ?
C12 Ir1 C11 88.49(17) 2_556 . ?
C12 Ir1 C1 91.51(17) . . ?
C12 Ir1 C1 91.51(17) 2_556 . ?
C11 Ir1 C1 180.0 . . ?
C12 Ir1 Cl1 177.08(18) . . ?
C11 Ir1 Cl1 88.74(4) . . ?
C1 Ir1 Cl1 91.26(4) . . ?
C12 Ir1 Cl1 177.08(18) 2_556 2_556 ?
C11 Ir1 Cl1 88.74(4) . 2_556 ?
C1 Ir1 Cl1 91.26(4) . 2_556 ?
Cl1 Ir1 Cl1 177.49(7) . 2_556 ?
O12 Cl1 C12 169.3(9) 2_556 2_556 ?
O12 Cl1 Ir1 171.4(7) 2_556 . ?
Cl1 C12 Ir1 176.0(9) 2_556 . ?
O12 C12 Ir1 176.6(6) . . ?
O11 C11 Ir1 180.0 . . ?
N2 C1 N2 108.8(3) 2_556 . ?
N2 C1 Ir1 125.59(15) 2_556 . ?
N2 C1 Ir1 125.59(15) . . ?
C1 N2 C21 126.7(2) . . ?
C1 N2 C3 111.6(2) . . ?
C21 N2 C3 120.6(2) . . ?
N2 C3 C3 101.84(19) . 2_556 ?
N2 C3 H3A 111.4 . . ?
C3 C3 H3A 111.4 2_556 . ?
N2 C3 H3B 111.4 . . ?
C3 C3 H3B 111.4 2_556 . ?
H3A C3 H3B 109.3 . . ?
C22 C21 C28A 121.5(2) . . ?
C22 C21 N2 118.8(2) . . ?
C28A C21 N2 119.3(2) . . ?
C21 C22 N221 121.6(2) . . ?
C21 C22 C23 117.8(2) . . ?
N221 C22 C23 120.5(2) . . ?
C24 C23 C22 121.7(2) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C24A 121.0(2) . . ?
C23 C24 H24 119.5 . . ?
C24A C24 H24 119.5 . . ?
C25 C24A C24 121.5(2) . . ?
C25 C24A C28A 119.8(2) . . ?
C24 C24A C28A 118.7(2) . . ?
C26 C25 C24A 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C24A C25 H25 119.7 . . ?
C25 C26 C27 120.1(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 121.0(3) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C21 C28A C24A 118.9(2) . . ?
C21 C28A C28 123.4(3) . . ?
C24A C28A C28 117.6(3) . . ?
C27 C28 C28A 120.8(3) . . ?
C27 C28 H28 119.6 . . ?
C28A C28 H28 119.6 . . ?
C22 N221 C222 117.3(2) . . ?
C22 N221 C226 116.1(2) . . ?
C222 N221 C226 111.4(3) . . ?
N221 C222 C223 110.3(2) . . ?
N221 C222 H22A 109.6 . . ?
C223 C222 H22A 109.6 . . ?
N221 C222 H22B 109.6 . . ?
C223 C222 H22B 109.6 . . ?
H22A C222 H22B 108.1 . . ?
C222 C223 C224 111.2(3) . . ?
C222 C223 H22C 109.4 . . ?
C224 C223 H22C 109.4 . . ?
C222 C223 H22D 109.4 . . ?
C224 C223 H22D 109.4 . . ?
H22C C223 H22D 108.0 . . ?
C223 C224 C225 109.7(4) . . ?
C223 C224 H22E 109.7 . . ?
C225 C224 H22E 109.7 . . ?
C223 C224 H22F 109.7 . . ?
C225 C224 H22F 109.7 . . ?
H22E C224 H22F 108.2 . . ?
C226 C225 C224 110.6(3) . . ?
C226 C225 H22G 109.5 . . ?
C224 C225 H22G 109.5 . . ?
C226 C225 H22H 109.5 . . ?
C224 C225 H22H 109.5 . . ?
H22G C225 H22H 108.1 . . ?
N221 C226 C225 109.6(3) . . ?
N221 C226 H22I 109.8 . . ?
C225 C226 H22I 109.8 . . ?
N221 C226 H22J 109.8 . . ?
C225 C226 H22J 109.8 . . ?
H22I C226 H22J 108.2 . . ?

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
N2 C1 N2 C21 -175.2(4) 2_556 . . . ?
Ir1 C1 N2 C21 4.8(4) . . . . ?
N2 C1 N2 C3 -7.1(2) 2_556 . . . ?
Ir1 C1 N2 C3 172.9(2) . . . . ?
C1 N2 C3 C3 17.4(6) . . . 2_556 ?
C21 N2 C3 C3 -173.7(4) . . . 2_556 ?
C1 N2 C21 C22 -122.3(3) . . . . ?
C3 N2 C21 C22 70.6(4) . . . . ?
C1 N2 C21 C28A 63.8(4) . . . . ?
C3 N2 C21 C28A -103.3(4) . . . . ?
C28A C21 C22 N221 170.1(2) . . . . ?
N2 C21 C22 N221 -3.7(4) . . . . ?
C28A C21 C22 C23 -6.5(4) . . . . ?
N2 C21 C22 C23 179.8(2) . . . . ?
C21 C22 C23 C24 1.3(4) . . . . ?
N221 C22 C23 C24 -175.3(2) . . . . ?
C22 C23 C24 C24A 3.2(4) . . . . ?
C23 C24 C24A C25 174.1(3) . . . . ?
C23 C24 C24A C28A -2.5(4) . . . . ?
C24 C24A C25 C26 -173.8(3) . . . . ?
C28A C24A C25 C26 2.8(4) . . . . ?
C24A C25 C26 C27 0.3(5) . . . . ?
C25 C26 C27 C28 -2.8(6) . . . . ?
C22 C21 C28A C24A 7.2(3) . . . . ?
N2 C21 C28A C24A -179.1(2) . . . . ?
C22 C21 C28A C28 -168.3(2) . . . . ?
N2 C21 C28A C28 5.4(4) . . . . ?
C25 C24A C28A C21 -179.3(2) . . . . ?
C24 C24A C28A C21 -2.6(3) . . . . ?
C25 C24A C28A C28 -3.5(3) . . . . ?
C24 C24A C28A C28 173.2(2) . . . . ?
C26 C27 C28 C28A 2.0(5) . . . . ?
C21 C28A C28 C27 176.7(3) . . . . ?
C24A C28A C28 C27 1.1(4) . . . . ?
C21 C22 N221 C222 69.9(4) . . . . ?
C23 C22 N221 C222 -113.6(3) . . . . ?
C21 C22 N221 C226 -154.8(3) . . . . ?
C23 C22 N221 C226 21.7(4) . . . . ?
C22 N221 C222 C223 -162.2(3) . . . . ?
C226 N221 C222 C223 60.5(4) . . . . ?
N221 C222 C223 C224 -57.3(5) . . . . ?
C222 C223 C224 C225 54.5(5) . . . . ?
C223 C224 C225 C226 -54.6(6) . . . . ?
C22 N221 C226 C225 161.7(3) . . . . ?
C222 N221 C226 C225 -60.5(4) . . . . ?
C224 C225 C226 N221 57.4(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3B N221 0.99 2.62 3.171(5) 115.1 .
C222 H22B Cl1 0.99 2.63 3.355(3) 129.9 2_556
C222 H22B N2 0.99 2.53 3.113(5) 117.5 .
C223 H22C Cl1 0.99 2.86 3.653(4) 138.0 8
C223 H22C O12 0.99 2.64 3.433(7) 137.0 7_556

_refine_diff_density_max         2.170
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.112

