# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

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

data_3c
_database_code_depnum_ccdc_archive 'CCDC 1865671'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2018-09-04 deposited with the CCDC.	2019-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H34'
_chemical_formula_weight         442.61

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   14.0303(19)
_cell_length_b                   23.979(4)
_cell_length_c                   7.3735(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.442(4)
_cell_angle_gamma                90
_cell_volume                     2473.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    123

_cell_measurement_reflns_used    2814

_cell_measurement_theta_min      3.1

_cell_measurement_theta_max      25.4


_exptl_crystal_description       Block

_exptl_crystal_colour            Colorless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15

_exptl_crystal_size_mid          0.10

_exptl_crystal_size_min          0.10

_exptl_absorpt_coefficient_mu    0.067
_shelx_estimated_absorpt_T_min   0.990
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.839

_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku CrystalClear-SM Expert 2.1 b29
;

_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_detector_area_resol_mean 5.8140

_diffrn_reflns_number            13626
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.146
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2188
_reflns_number_gt                1869
_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       
;
Rigaku CrystalClear-SM Expert 2.1 b29
;
_computing_cell_refinement       
;
Rigaku CrystalClear-SM Expert 2.1 b29
;
_computing_data_reduction        
;
Rigaku CrystalClear-SM Expert 2.1 b29
;
_computing_structure_solution    SIR-97

_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.0488P)²+1.2487P] 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         2188
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0913
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.52024(9) 0.06100(5) 0.67031(17) 0.0294(3) Uani 1 1 d . . . . .
H1 H 0.530710 0.026577 0.611224 0.035 Uiso 1 1 calc R U . . .
C2 C 0.54786(8) 0.11209(5) 0.58800(16) 0.0250(3) Uani 1 1 d . . . . .
C3 C 0.53191(8) 0.16373(5) 0.67575(15) 0.0205(3) Uani 1 1 d . . . . .
C4 C 0.58349(8) 0.21118(5) 0.61785(15) 0.0210(3) Uani 1 1 d . . . . .
C5 C 0.63039(8) 0.20739(5) 0.45932(16) 0.0256(3) Uani 1 1 d . . . . .
H2 H 0.661569 0.239530 0.417295 0.031 Uiso 1 1 calc R U . . .
C6 C 0.63341(9) 0.15809(5) 0.35948(16) 0.0290(3) Uani 1 1 d . . . . .
H3 H 0.661163 0.157539 0.245998 0.035 Uiso 1 1 calc R U . . .
C7 C 0.59582(9) 0.11061(5) 0.42744(16) 0.0286(3) Uani 1 1 d . . . . .
H4 H 0.602144 0.076213 0.365595 0.034 Uiso 1 1 calc R U . . .
C8 C 0.60103(8) 0.26247(5) 0.72937(15) 0.0199(3) Uani 1 1 d . . . . .
C9 C 0.62653(8) 0.25930(5) 0.91525(15) 0.0215(3) Uani 1 1 d . . . . .
H5 H 0.627978 0.223979 0.973752 0.026 Uiso 1 1 calc R U . . .
C10 C 0.64985(8) 0.30673(5) 1.01662(15) 0.0216(3) Uani 1 1 d . . . . .
H6 H 0.666702 0.303143 1.143369 0.026 Uiso 1 1 calc R U . . .
C11 C 0.64924(8) 0.35954(5) 0.93756(15) 0.0203(3) Uani 1 1 d . . . . .
C12 C 0.62462(8) 0.36231(5) 0.75025(15) 0.0214(3) Uani 1 1 d . . . . .
H7 H 0.624045 0.397556 0.691308 0.026 Uiso 1 1 calc R U . . .
C13 C 0.60116(8) 0.31527(5) 0.64890(15) 0.0209(3) Uani 1 1 d . . . . .
H8 H 0.584781 0.318792 0.521977 0.025 Uiso 1 1 calc R U . . .
C14 C 0.67438(8) 0.41277(5) 1.04588(15) 0.0230(3) Uani 1 1 d . . . . .
C15 C 0.69384(10) 0.40145(5) 1.24927(17) 0.0328(3) Uani 1 1 d . . . . .
H9 H 0.636720 0.385223 1.296889 0.049 Uiso 1 1 calc R U . . .
H10 H 0.709871 0.436514 1.312754 0.049 Uiso 1 1 calc R U . . .
H11 H 0.747402 0.375344 1.268642 0.049 Uiso 1 1 calc R U . . .
C16 C 0.76391(9) 0.43955(5) 0.97531(18) 0.0322(3) Uani 1 1 d . . . . .
H12 H 0.818359 0.414164 0.996674 0.048 Uiso 1 1 calc R U . . .
H13 H 0.777837 0.474736 1.039625 0.048 Uiso 1 1 calc R U . . .
H14 H 0.752631 0.446839 0.844629 0.048 Uiso 1 1 calc R U . . .
C17 C 0.59092(9) 0.45392(5) 1.02083(17) 0.0291(3) Uani 1 1 d . . . . .
H15 H 0.578245 0.462572 0.891315 0.044 Uiso 1 1 calc R U . . .
H16 H 0.607310 0.488277 1.088153 0.044 Uiso 1 1 calc R U . . .
H17 H 0.533800 0.437236 1.066995 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.344(3) 2_656 ?
C1 C2 1.4340(17) . ?
C1 H1 0.9500 . ?
C2 C7 1.4068(18) . ?
C2 C3 1.4228(16) . ?
C3 C4 1.4311(16) . ?
C3 C3 1.467(2) 2_656 ?
C4 C5 1.3880(17) . ?
C4 C8 1.4894(16) . ?
C5 C6 1.3950(17) . ?
C5 H2 0.9500 . ?
C6 C7 1.3660(18) . ?
C6 H3 0.9500 . ?
C7 H4 0.9500 . ?
C8 C9 1.3915(16) . ?
C8 C13 1.3982(16) . ?
C9 C10 1.3861(16) . ?
C9 H5 0.9500 . ?
C10 C11 1.3938(16) . ?
C10 H6 0.9500 . ?
C11 C12 1.3991(16) . ?
C11 C14 1.5324(15) . ?
C12 C13 1.3789(16) . ?
C12 H7 0.9500 . ?
C13 H8 0.9500 . ?
C14 C15 1.5277(17) . ?
C14 C17 1.5314(16) . ?
C14 C16 1.5371(17) . ?
C15 H9 0.9800 . ?
C15 H10 0.9800 . ?
C15 H11 0.9800 . ?
C16 H12 0.9800 . ?
C16 H13 0.9800 . ?
C16 H14 0.9800 . ?
C17 H15 0.9800 . ?
C17 H16 0.9800 . ?
C17 H17 0.9800 . ?

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 C1 C2 121.09(7) 2_656 . ?
C1 C1 H1 119.5 2_656 . ?
C2 C1 H1 119.5 . . ?
C7 C2 C3 120.46(11) . . ?
C7 C2 C1 119.81(11) . . ?
C3 C2 C1 119.61(11) . . ?
C2 C3 C4 117.08(11) . . ?
C2 C3 C3 117.77(7) . 2_656 ?
C4 C3 C3 125.07(7) . 2_656 ?
C5 C4 C3 118.87(11) . . ?
C5 C4 C8 116.75(10) . . ?
C3 C4 C8 123.88(10) . . ?
C4 C5 C6 122.39(12) . . ?
C4 C5 H2 118.8 . . ?
C6 C5 H2 118.8 . . ?
C7 C6 C5 118.96(11) . . ?
C7 C6 H3 120.5 . . ?
C5 C6 H3 120.5 . . ?
C6 C7 C2 120.74(11) . . ?
C6 C7 H4 119.6 . . ?
C2 C7 H4 119.6 . . ?
C9 C8 C13 117.31(10) . . ?
C9 C8 C4 121.17(10) . . ?
C13 C8 C4 121.27(10) . . ?
C10 C9 C8 121.22(10) . . ?
C10 C9 H5 119.4 . . ?
C8 C9 H5 119.4 . . ?
C9 C10 C11 121.76(10) . . ?
C9 C10 H6 119.1 . . ?
C11 C10 H6 119.1 . . ?
C10 C11 C12 116.69(10) . . ?
C10 C11 C14 123.03(10) . . ?
C12 C11 C14 120.28(10) . . ?
C13 C12 C11 121.76(10) . . ?
C13 C12 H7 119.1 . . ?
C11 C12 H7 119.1 . . ?
C12 C13 C8 121.26(10) . . ?
C12 C13 H8 119.4 . . ?
C8 C13 H8 119.4 . . ?
C15 C14 C17 108.05(10) . . ?
C15 C14 C11 112.33(10) . . ?
C17 C14 C11 109.32(9) . . ?
C15 C14 C16 108.54(10) . . ?
C17 C14 C16 109.11(10) . . ?
C11 C14 C16 109.43(9) . . ?
C14 C15 H9 109.5 . . ?
C14 C15 H10 109.5 . . ?
H9 C15 H10 109.5 . . ?
C14 C15 H11 109.5 . . ?
H9 C15 H11 109.5 . . ?
H10 C15 H11 109.5 . . ?
C14 C16 H12 109.5 . . ?
C14 C16 H13 109.5 . . ?
H12 C16 H13 109.5 . . ?
C14 C16 H14 109.5 . . ?
H12 C16 H14 109.5 . . ?
H13 C16 H14 109.5 . . ?
C14 C17 H15 109.5 . . ?
C14 C17 H16 109.5 . . ?
H15 C17 H16 109.5 . . ?
C14 C17 H17 109.5 . . ?
H15 C17 H17 109.5 . . ?
H16 C17 H17 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C7 175.76(14) 2_656 . . . ?
C1 C1 C2 C3 -0.3(2) 2_656 . . . ?
C7 C2 C3 C4 -13.05(16) . . . . ?
C1 C2 C3 C4 162.95(10) . . . . ?
C7 C2 C3 C3 170.05(12) . . . 2_656 ?
C1 C2 C3 C3 -13.96(18) . . . 2_656 ?
C2 C3 C4 C5 12.51(15) . . . . ?
C3 C3 C4 C5 -170.83(12) 2_656 . . . ?
C2 C3 C4 C8 -159.18(10) . . . . ?
C3 C3 C4 C8 17.47(19) 2_656 . . . ?
C3 C4 C5 C6 -3.52(17) . . . . ?
C8 C4 C5 C6 168.76(10) . . . . ?
C4 C5 C6 C7 -5.55(18) . . . . ?
C5 C6 C7 C2 5.13(18) . . . . ?
C3 C2 C7 C6 4.32(17) . . . . ?
C1 C2 C7 C6 -171.66(11) . . . . ?
C5 C4 C8 C9 -129.93(12) . . . . ?
C3 C4 C8 C9 41.93(16) . . . . ?
C5 C4 C8 C13 44.11(15) . . . . ?
C3 C4 C8 C13 -144.04(11) . . . . ?
C13 C8 C9 C10 0.83(16) . . . . ?
C4 C8 C9 C10 175.10(10) . . . . ?
C8 C9 C10 C11 -0.25(17) . . . . ?
C9 C10 C11 C12 -0.49(16) . . . . ?
C9 C10 C11 C14 179.82(10) . . . . ?
C10 C11 C12 C13 0.63(16) . . . . ?
C14 C11 C12 C13 -179.67(10) . . . . ?
C11 C12 C13 C8 -0.04(17) . . . . ?
C9 C8 C13 C12 -0.69(16) . . . . ?
C4 C8 C13 C12 -174.95(10) . . . . ?
C10 C11 C14 C15 -3.45(15) . . . . ?
C12 C11 C14 C15 176.87(10) . . . . ?
C10 C11 C14 C17 -123.38(12) . . . . ?
C12 C11 C14 C17 56.94(13) . . . . ?
C10 C11 C14 C16 117.18(12) . . . . ?
C12 C11 C14 C16 -62.50(13) . . . . ?

_refine_diff_density_max         0.172
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.033


_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  Confocal
_chemical_absolute_configuration unk
####################################################################### 
# 
# 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_3t
_database_code_depnum_ccdc_archive 'CCDC 1865672'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2018-09-04 deposited with the CCDC.	2019-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H26'
_chemical_formula_weight         482.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.9305(2)
_cell_length_b                   16.0425(3)
_cell_length_c                   18.2272(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.3021(19)
_cell_angle_gamma                90
_cell_volume                     2560.73(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)

_cell_measurement_reflns_used    13416

_cell_measurement_theta_min      2.2620

_cell_measurement_theta_max      27.7570


_exptl_crystal_description       block

_exptl_crystal_colour            colorless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   0.989
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.84888

_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      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            22958
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.279
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4498
_reflns_number_gt                3965
_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    SIR97

_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.0438P)²+0.6568P] 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         4498
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.64093(13) 0.08737(7) 0.12221(6) 0.0210(2) Uani 1 1 d . . . . .
C2 C 0.68814(12) 0.07729(6) 0.19976(6) 0.0184(2) Uani 1 1 d . . . . .
C3 C 0.58733(12) 0.03734(6) 0.24142(6) 0.0188(2) Uani 1 1 d . . . . .
C4 C 0.61847(12) 0.02686(6) 0.32340(6) 0.0187(2) Uani 1 1 d . . . . .
C5 C 0.69782(12) 0.08531(7) 0.37662(6) 0.0181(2) Uani 1 1 d . . . . .
C6 C 0.73543(12) 0.06292(7) 0.45242(6) 0.0204(2) Uani 1 1 d . . . . .
C7 C 0.69769(13) -0.01672(7) 0.47568(6) 0.0248(3) Uani 1 1 d . . . . .
H1 H 0.736271 -0.034549 0.525500 0.030 Uiso 1 1 calc R U . . .
C8 C 0.60601(13) -0.06840(7) 0.42702(6) 0.0260(3) Uani 1 1 d . . . . .
H2 H 0.574718 -0.120250 0.444219 0.031 Uiso 1 1 calc R U . . .
C9 C 0.55735(13) -0.04563(7) 0.35158(6) 0.0221(2) Uani 1 1 d . . . . .
C10 C 0.43703(14) -0.09154(7) 0.30526(7) 0.0263(3) Uani 1 1 d . . . . .
H3 H 0.397826 -0.140296 0.324295 0.032 Uiso 1 1 calc R U . . .
C11 C 0.37920(13) -0.06627(7) 0.23521(7) 0.0259(3) Uani 1 1 d . . . . .
H4 H 0.287556 -0.090513 0.208446 0.031 Uiso 1 1 calc R U . . .
C12 C 0.45485(12) -0.00295(7) 0.20053(6) 0.0216(2) Uani 1 1 d . . . . .
C13 C 0.40682(13) 0.01323(7) 0.12365(6) 0.0246(3) Uani 1 1 d . . . . .
H5 H 0.312320 -0.008593 0.097656 0.030 Uiso 1 1 calc R U . . .
C14 C 0.49502(13) 0.06008(7) 0.08611(6) 0.0241(3) Uani 1 1 d . . . . .
H6 H 0.457721 0.074390 0.035236 0.029 Uiso 1 1 calc R U . . .
C15 C 0.74138(13) 0.11871(7) 0.07134(6) 0.0228(2) Uani 1 1 d . . . . .
C16 C 0.69167(14) 0.18408(8) 0.02222(6) 0.0284(3) Uani 1 1 d . . . . .
H7 H 0.598621 0.211728 0.024491 0.034 Uiso 1 1 calc R U . . .
C17 C 0.77668(16) 0.20926(8) -0.03003(7) 0.0346(3) Uani 1 1 d . . . . .
H8 H 0.742015 0.254236 -0.062896 0.042 Uiso 1 1 calc R U . . .
C18 C 0.91130(15) 0.16914(8) -0.03432(7) 0.0353(3) Uani 1 1 d . . . . .
H9 H 0.968647 0.185855 -0.070535 0.042 Uiso 1 1 calc R U . . .
C19 C 0.96251(15) 0.10436(8) 0.01441(7) 0.0337(3) Uani 1 1 d . . . . .
H10 H 1.055816 0.077085 0.011928 0.040 Uiso 1 1 calc R U . . .
C20 C 0.87820(14) 0.07909(8) 0.06683(6) 0.0278(3) Uani 1 1 d . . . . .
H11 H 0.914004 0.034456 0.099891 0.033 Uiso 1 1 calc R U . . .
C21 C 0.85109(12) 0.09489(7) 0.23464(6) 0.0191(2) Uani 1 1 d . . . . .
C22 C 0.92383(13) 0.16929(7) 0.22259(6) 0.0232(2) Uani 1 1 d . . . . .
H12 H 0.866677 0.213093 0.195292 0.028 Uiso 1 1 calc R U . . .
C23 C 1.07879(14) 0.17975(8) 0.25015(7) 0.0293(3) Uani 1 1 d . . . . .
H13 H 1.126985 0.230673 0.241694 0.035 Uiso 1 1 calc R U . . .
C24 C 1.16380(14) 0.11634(8) 0.28996(7) 0.0316(3) Uani 1 1 d . . . . .
H14 H 1.270183 0.123501 0.308195 0.038 Uiso 1 1 calc R U . . .
C25 C 1.09307(13) 0.04258(8) 0.30303(7) 0.0270(3) Uani 1 1 d . . . . .
H15 H 1.150621 -0.000824 0.330744 0.032 Uiso 1 1 calc R U . . .
C26 C 0.93813(12) 0.03212(7) 0.27562(6) 0.0208(2) Uani 1 1 d . . . . .
H16 H 0.890340 -0.018655 0.284889 0.025 Uiso 1 1 calc R U . . .
C27 C 0.72263(12) 0.17397(6) 0.35655(5) 0.0177(2) Uani 1 1 d . . . . .
C28 C 0.59955(13) 0.22150(7) 0.32036(6) 0.0200(2) Uani 1 1 d . . . . .
H17 H 0.503562 0.195421 0.303208 0.024 Uiso 1 1 calc R U . . .
C29 C 0.61496(13) 0.30647(7) 0.30895(6) 0.0234(2) Uani 1 1 d . . . . .
H18 H 0.529613 0.338060 0.284577 0.028 Uiso 1 1 calc R U . . .
C30 C 0.75439(14) 0.34511(7) 0.33304(6) 0.0258(3) Uani 1 1 d . . . . .
H19 H 0.764838 0.403330 0.325945 0.031 Uiso 1 1 calc R U . . .
C31 C 0.87879(14) 0.29825(7) 0.36762(6) 0.0246(3) Uani 1 1 d . . . . .
H20 H 0.975366 0.324255 0.383178 0.030 Uiso 1 1 calc R U . . .
C32 C 0.86302(13) 0.21371(7) 0.37961(6) 0.0213(2) Uani 1 1 d . . . . .
H21 H 0.948852 0.182386 0.403843 0.026 Uiso 1 1 calc R U . . .
C33 C 0.80182(13) 0.12312(7) 0.51281(6) 0.0211(2) Uani 1 1 d . . . . .
C34 C 0.94400(14) 0.10913(7) 0.55852(6) 0.0263(3) Uani 1 1 d . . . . .
H22 H 1.002129 0.061631 0.550350 0.032 Uiso 1 1 calc R U . . .
C35 C 1.00116(15) 0.16423(8) 0.61594(7) 0.0316(3) Uani 1 1 d . . . . .
H23 H 1.098934 0.154703 0.646288 0.038 Uiso 1 1 calc R U . . .
C36 C 0.91674(15) 0.23288(7) 0.62924(6) 0.0310(3) Uani 1 1 d . . . . .
H24 H 0.956146 0.270266 0.668731 0.037 Uiso 1 1 calc R U . . .
C37 C 0.77444(15) 0.24694(7) 0.58473(6) 0.0279(3) Uani 1 1 d . . . . .
H25 H 0.715725 0.293819 0.593859 0.034 Uiso 1 1 calc R U . . .
C38 C 0.71790(13) 0.19254(7) 0.52691(6) 0.0234(2) Uani 1 1 d . . . . .
H26 H 0.620495 0.202683 0.496421 0.028 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
C1 C2 1.4030(15) . ?
C1 C14 1.4095(16) . ?
C1 C15 1.4977(15) . ?
C2 C3 1.4373(15) . ?
C2 C21 1.4963(15) . ?
C3 C12 1.4239(15) . ?
C3 C4 1.4750(15) . ?
C4 C9 1.4227(15) . ?
C4 C5 1.4327(15) . ?
C5 C6 1.4032(15) . ?
C5 C27 1.4959(14) . ?
C6 C7 1.4077(16) . ?
C6 C33 1.4966(15) . ?
C7 C8 1.3638(16) . ?
C7 H1 0.9500 . ?
C8 C9 1.4067(16) . ?
C8 H2 0.9500 . ?
C9 C10 1.4332(16) . ?
C10 C11 1.3427(17) . ?
C10 H3 0.9500 . ?
C11 C12 1.4335(16) . ?
C11 H4 0.9500 . ?
C12 C13 1.4070(16) . ?
C13 C14 1.3655(17) . ?
C13 H5 0.9500 . ?
C14 H6 0.9500 . ?
C15 C16 1.3938(16) . ?
C15 C20 1.3940(17) . ?
C16 C17 1.3892(17) . ?
C16 H7 0.9500 . ?
C17 C18 1.379(2) . ?
C17 H8 0.9500 . ?
C18 C19 1.3852(19) . ?
C18 H9 0.9500 . ?
C19 C20 1.3879(17) . ?
C19 H10 0.9500 . ?
C20 H11 0.9500 . ?
C21 C26 1.3959(15) . ?
C21 C22 1.3967(15) . ?
C22 C23 1.3868(17) . ?
C22 H12 0.9500 . ?
C23 C24 1.3861(18) . ?
C23 H13 0.9500 . ?
C24 C25 1.3838(17) . ?
C24 H14 0.9500 . ?
C25 C26 1.3861(16) . ?
C25 H15 0.9500 . ?
C26 H16 0.9500 . ?
C27 C28 1.3930(15) . ?
C27 C32 1.3959(15) . ?
C28 C29 1.3898(16) . ?
C28 H17 0.9500 . ?
C29 C30 1.3832(16) . ?
C29 H18 0.9500 . ?
C30 C31 1.3864(17) . ?
C30 H19 0.9500 . ?
C31 C32 1.3852(16) . ?
C31 H20 0.9500 . ?
C32 H21 0.9500 . ?
C33 C34 1.3936(16) . ?
C33 C38 1.3942(16) . ?
C34 C35 1.3885(17) . ?
C34 H22 0.9500 . ?
C35 C36 1.3826(18) . ?
C35 H23 0.9500 . ?
C36 C37 1.3856(18) . ?
C36 H24 0.9500 . ?
C37 C38 1.3851(16) . ?
C37 H25 0.9500 . ?
C38 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 120.15(10) . . ?
C2 C1 C15 124.35(10) . . ?
C14 C1 C15 115.24(9) . . ?
C1 C2 C3 119.21(10) . . ?
C1 C2 C21 118.79(9) . . ?
C3 C2 C21 121.15(9) . . ?
C12 C3 C2 117.91(9) . . ?
C12 C3 C4 116.80(9) . . ?
C2 C3 C4 124.94(9) . . ?
C9 C4 C5 117.67(9) . . ?
C9 C4 C3 116.70(9) . . ?
C5 C4 C3 125.54(9) . . ?
C6 C5 C4 119.36(10) . . ?
C6 C5 C27 117.76(9) . . ?
C4 C5 C27 122.28(9) . . ?
C5 C6 C7 120.24(10) . . ?
C5 C6 C33 122.88(10) . . ?
C7 C6 C33 116.61(9) . . ?
C8 C7 C6 120.30(10) . . ?
C8 C7 H1 119.8 . . ?
C6 C7 H1 119.8 . . ?
C7 C8 C9 120.59(10) . . ?
C7 C8 H2 119.7 . . ?
C9 C8 H2 119.7 . . ?
C8 C9 C4 119.89(10) . . ?
C8 C9 C10 119.65(10) . . ?
C4 C9 C10 120.25(10) . . ?
C11 C10 C9 120.62(10) . . ?
C11 C10 H3 119.7 . . ?
C9 C10 H3 119.7 . . ?
C10 C11 C12 120.43(10) . . ?
C10 C11 H4 119.8 . . ?
C12 C11 H4 119.8 . . ?
C13 C12 C3 119.83(10) . . ?
C13 C12 C11 119.46(10) . . ?
C3 C12 C11 120.39(10) . . ?
C14 C13 C12 120.49(10) . . ?
C14 C13 H5 119.8 . . ?
C12 C13 H5 119.8 . . ?
C13 C14 C1 120.56(10) . . ?
C13 C14 H6 119.7 . . ?
C1 C14 H6 119.7 . . ?
C16 C15 C20 118.54(11) . . ?
C16 C15 C1 119.75(10) . . ?
C20 C15 C1 121.44(10) . . ?
C17 C16 C15 120.74(12) . . ?
C17 C16 H7 119.6 . . ?
C15 C16 H7 119.6 . . ?
C18 C17 C16 120.17(12) . . ?
C18 C17 H8 119.9 . . ?
C16 C17 H8 119.9 . . ?
C17 C18 C19 119.72(11) . . ?
C17 C18 H9 120.1 . . ?
C19 C18 H9 120.1 . . ?
C18 C19 C20 120.33(12) . . ?
C18 C19 H10 119.8 . . ?
C20 C19 H10 119.8 . . ?
C19 C20 C15 120.49(12) . . ?
C19 C20 H11 119.8 . . ?
C15 C20 H11 119.8 . . ?
C26 C21 C22 118.24(10) . . ?
C26 C21 C2 118.98(9) . . ?
C22 C21 C2 122.55(10) . . ?
C23 C22 C21 120.55(11) . . ?
C23 C22 H12 119.7 . . ?
C21 C22 H12 119.7 . . ?
C24 C23 C22 120.40(11) . . ?
C24 C23 H13 119.8 . . ?
C22 C23 H13 119.8 . . ?
C25 C24 C23 119.73(11) . . ?
C25 C24 H14 120.1 . . ?
C23 C24 H14 120.1 . . ?
C24 C25 C26 119.91(11) . . ?
C24 C25 H15 120.0 . . ?
C26 C25 H15 120.0 . . ?
C25 C26 C21 121.16(10) . . ?
C25 C26 H16 119.4 . . ?
C21 C26 H16 119.4 . . ?
C28 C27 C32 118.12(10) . . ?
C28 C27 C5 119.69(9) . . ?
C32 C27 C5 121.87(10) . . ?
C29 C28 C27 121.04(10) . . ?
C29 C28 H17 119.5 . . ?
C27 C28 H17 119.5 . . ?
C30 C29 C28 120.10(10) . . ?
C30 C29 H18 120.0 . . ?
C28 C29 H18 120.0 . . ?
C29 C30 C31 119.51(10) . . ?
C29 C30 H19 120.2 . . ?
C31 C30 H19 120.2 . . ?
C32 C31 C30 120.36(10) . . ?
C32 C31 H20 119.8 . . ?
C30 C31 H20 119.8 . . ?
C31 C32 C27 120.85(10) . . ?
C31 C32 H21 119.6 . . ?
C27 C32 H21 119.6 . . ?
C34 C33 C38 118.57(10) . . ?
C34 C33 C6 121.26(10) . . ?
C38 C33 C6 120.09(10) . . ?
C35 C34 C33 120.36(11) . . ?
C35 C34 H22 119.8 . . ?
C33 C34 H22 119.8 . . ?
C36 C35 C34 120.45(12) . . ?
C36 C35 H23 119.8 . . ?
C34 C35 H23 119.8 . . ?
C35 C36 C37 119.74(11) . . ?
C35 C36 H24 120.1 . . ?
C37 C36 H24 120.1 . . ?
C38 C37 C36 119.91(11) . . ?
C38 C37 H25 120.0 . . ?
C36 C37 H25 120.0 . . ?
C37 C38 C33 120.97(11) . . ?
C37 C38 H26 119.5 . . ?
C33 C38 H26 119.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 1.29(15) . . . . ?
C15 C1 C2 C3 -172.57(10) . . . . ?
C14 C1 C2 C21 170.88(10) . . . . ?
C15 C1 C2 C21 -2.97(15) . . . . ?
C1 C2 C3 C12 10.54(14) . . . . ?
C21 C2 C3 C12 -158.80(9) . . . . ?
C1 C2 C3 C4 -176.41(10) . . . . ?
C21 C2 C3 C4 14.24(15) . . . . ?
C12 C3 C4 C9 24.95(14) . . . . ?
C2 C3 C4 C9 -148.17(10) . . . . ?
C12 C3 C4 C5 -151.68(10) . . . . ?
C2 C3 C4 C5 35.21(16) . . . . ?
C9 C4 C5 C6 11.01(15) . . . . ?
C3 C4 C5 C6 -172.40(10) . . . . ?
C9 C4 C5 C27 -159.91(10) . . . . ?
C3 C4 C5 C27 16.69(16) . . . . ?
C4 C5 C6 C7 1.04(16) . . . . ?
C27 C5 C6 C7 172.36(10) . . . . ?
C4 C5 C6 C33 -172.76(10) . . . . ?
C27 C5 C6 C33 -1.43(15) . . . . ?
C5 C6 C7 C8 -9.23(17) . . . . ?
C33 C6 C7 C8 164.94(10) . . . . ?
C6 C7 C8 C9 4.85(17) . . . . ?
C7 C8 C9 C4 7.66(17) . . . . ?
C7 C8 C9 C10 -167.02(11) . . . . ?
C5 C4 C9 C8 -15.40(15) . . . . ?
C3 C4 C9 C8 167.70(10) . . . . ?
C5 C4 C9 C10 159.24(10) . . . . ?
C3 C4 C9 C10 -17.66(15) . . . . ?
C8 C9 C10 C11 173.81(11) . . . . ?
C4 C9 C10 C11 -0.85(17) . . . . ?
C9 C10 C11 C12 11.92(17) . . . . ?
C2 C3 C12 C13 -14.83(15) . . . . ?
C4 C3 C12 C13 171.56(10) . . . . ?
C2 C3 C12 C11 158.69(10) . . . . ?
C4 C3 C12 C11 -14.92(14) . . . . ?
C10 C11 C12 C13 169.89(11) . . . . ?
C10 C11 C12 C3 -3.65(16) . . . . ?
C3 C12 C13 C14 7.16(16) . . . . ?
C11 C12 C13 C14 -166.41(10) . . . . ?
C12 C13 C14 C1 5.11(17) . . . . ?
C2 C1 C14 C13 -9.37(16) . . . . ?
C15 C1 C14 C13 165.02(10) . . . . ?
C2 C1 C15 C16 -128.78(12) . . . . ?
C14 C1 C15 C16 57.10(14) . . . . ?
C2 C1 C15 C20 57.21(15) . . . . ?
C14 C1 C15 C20 -116.91(12) . . . . ?
C20 C15 C16 C17 -0.07(17) . . . . ?
C1 C15 C16 C17 -174.25(10) . . . . ?
C15 C16 C17 C18 0.57(18) . . . . ?
C16 C17 C18 C19 -0.90(18) . . . . ?
C17 C18 C19 C20 0.75(18) . . . . ?
C18 C19 C20 C15 -0.25(18) . . . . ?
C16 C15 C20 C19 -0.09(17) . . . . ?
C1 C15 C20 C19 173.99(11) . . . . ?
C1 C2 C21 C26 -122.76(11) . . . . ?
C3 C2 C21 C26 46.63(14) . . . . ?
C1 C2 C21 C22 51.60(14) . . . . ?
C3 C2 C21 C22 -139.01(11) . . . . ?
C26 C21 C22 C23 0.63(16) . . . . ?
C2 C21 C22 C23 -173.77(10) . . . . ?
C21 C22 C23 C24 0.13(17) . . . . ?
C22 C23 C24 C25 -0.80(18) . . . . ?
C23 C24 C25 C26 0.68(18) . . . . ?
C24 C25 C26 C21 0.10(17) . . . . ?
C22 C21 C26 C25 -0.75(15) . . . . ?
C2 C21 C26 C25 173.85(10) . . . . ?
C6 C5 C27 C28 -120.49(11) . . . . ?
C4 C5 C27 C28 50.56(14) . . . . ?
C6 C5 C27 C32 52.92(14) . . . . ?
C4 C5 C27 C32 -136.02(11) . . . . ?
C32 C27 C28 C29 -1.40(15) . . . . ?
C5 C27 C28 C29 172.25(10) . . . . ?
C27 C28 C29 C30 0.57(16) . . . . ?
C28 C29 C30 C31 0.90(16) . . . . ?
C29 C30 C31 C32 -1.51(16) . . . . ?
C30 C31 C32 C27 0.67(16) . . . . ?
C28 C27 C32 C31 0.78(15) . . . . ?
C5 C27 C32 C31 -172.73(10) . . . . ?
C5 C6 C33 C34 -120.32(12) . . . . ?
C7 C6 C33 C34 65.68(14) . . . . ?
C5 C6 C33 C38 63.11(14) . . . . ?
C7 C6 C33 C38 -110.89(12) . . . . ?
C38 C33 C34 C35 -1.09(16) . . . . ?
C6 C33 C34 C35 -177.71(10) . . . . ?
C33 C34 C35 C36 1.05(18) . . . . ?
C34 C35 C36 C37 -0.28(18) . . . . ?
C35 C36 C37 C38 -0.41(17) . . . . ?
C36 C37 C38 C33 0.35(17) . . . . ?
C34 C33 C38 C37 0.40(16) . . . . ?
C6 C33 C38 C37 177.06(10) . . . . ?

_refine_diff_density_max         0.160
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.034


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration unk
####################################################################### 
# 
# 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_3w
_database_code_depnum_ccdc_archive 'CCDC 1865673'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2018-09-04 deposited with the CCDC.	2019-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C101.50 H73.50 Cl7 O0.50 P4 Pd2'
_chemical_formula_weight         1885.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 '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                   14.5697(2)
_cell_length_b                   14.7169(2)
_cell_length_c                   23.7580(4)
_cell_angle_alpha                92.5220(10)
_cell_angle_beta                 105.129(2)
_cell_angle_gamma                116.309(2)
_cell_volume                     4332.56(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_cell_measurement_reflns_used    23772

_cell_measurement_theta_min      2.5970

_cell_measurement_theta_max      30.4440


_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             1915
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.754
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.81732

_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      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            47820
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.604
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             15188
_reflns_number_gt                12582
_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    SHELXT

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.0511P)²+7.4531P] 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         15188
_refine_ls_number_parameters     1046
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0989
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.032
_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
Pd1 Pd 0.75024(2) 0.30723(2) 0.64029(2) 0.02012(7) Uani 1 1 d . . . . .
P1 P 0.92828(7) 0.35358(6) 0.69394(4) 0.02128(19) Uani 1 1 d . . . . .
C1 C 0.9539(3) 0.2572(2) 0.73062(15) 0.0214(7) Uani 1 1 d . . . . .
C2 C 0.9464(3) 0.1736(2) 0.69584(15) 0.0224(7) Uani 1 1 d . . . . .
H1 H 0.9285 0.1683 0.6540 0.027 Uiso 1 1 calc R U . . .
C3 C 0.9649(3) 0.0988(3) 0.72191(16) 0.0241(7) Uani 1 1 d . . . . .
H2 H 0.9606 0.0429 0.6978 0.029 Uiso 1 1 calc R U . . .
C4 C 0.9898(3) 0.1041(3) 0.78333(16) 0.0252(8) Uani 1 1 d . . . . .
C5 C 0.9973(3) 0.1882(3) 0.81793(16) 0.0264(8) Uani 1 1 d . . . . .
H3 H 1.0143 0.1933 0.8598 0.032 Uiso 1 1 calc R U . . .
C6 C 0.9801(3) 0.2635(3) 0.79181(15) 0.0249(7) Uani 1 1 d . . . . .
H4 H 0.9861 0.3204 0.8159 0.030 Uiso 1 1 calc R U . . .
C7 C 1.0173(3) 0.0271(3) 0.81152(16) 0.0277(8) Uani 1 1 d . . . . .
C8 C 1.1101(3) 0.0652(3) 0.85964(18) 0.0363(9) Uani 1 1 d . . . . .
H5 H 1.1440 0.1359 0.8776 0.044 Uiso 1 1 calc R U . . .
C9 C 1.1553(3) 0.0043(3) 0.8826(2) 0.0435(10) Uani 1 1 d . . . . .
H6 H 1.2148 0.0305 0.9180 0.052 Uiso 1 1 calc R U . . .
C10 C 1.1122(4) -0.0943(4) 0.8531(2) 0.0443(11) Uani 1 1 d . . . . .
H7 H 1.1471 -0.1345 0.8659 0.053 Uiso 1 1 calc R U . . .
C11 C 1.0170(3) -0.1380(3) 0.80418(18) 0.0372(10) Uani 1 1 d . . . . .
C12 C 0.9800(4) -0.2367(3) 0.7707(2) 0.0454(11) Uani 1 1 d . . . . .
H8 H 1.0165 -0.2756 0.7833 0.055 Uiso 1 1 calc R U . . .
C13 C 0.8951(4) -0.2754(3) 0.7219(2) 0.0456(11) Uani 1 1 d . . . . .
H9 H 0.8788 -0.3362 0.6968 0.055 Uiso 1 1 calc R U . . .
C14 C 0.8271(3) -0.2272(3) 0.70625(18) 0.0376(10) Uani 1 1 d . . . . .
C15 C 0.7307(4) -0.2763(3) 0.65862(19) 0.0460(11) Uani 1 1 d . . . . .
H10 H 0.7150 -0.3371 0.6337 0.055 Uiso 1 1 calc R U . . .
C16 C 0.6601(4) -0.2380(3) 0.64781(19) 0.0496(12) Uani 1 1 d . . . . .
H11 H 0.5978 -0.2686 0.6138 0.059 Uiso 1 1 calc R U . . .
C17 C 0.6794(3) -0.1532(3) 0.68701(17) 0.0390(10) Uani 1 1 d . . . . .
H12 H 0.6272 -0.1294 0.6807 0.047 Uiso 1 1 calc R U . . .
C18 C 0.7732(3) -0.1028(3) 0.73503(16) 0.0280(8) Uani 1 1 d . . . . .
C19 C 0.8548(3) -0.1337(3) 0.74240(16) 0.0288(8) Uani 1 1 d . . . . .
C20 C 0.9617(3) -0.0803(3) 0.78627(16) 0.0275(8) Uani 1 1 d . . . . .
C21 C 0.7724(3) -0.0302(3) 0.78019(15) 0.0255(8) Uani 1 1 d . . . . .
C22 C 0.8018(3) -0.0377(3) 0.84019(15) 0.0265(8) Uani 1 1 d . . . . .
H23 H 0.8298 -0.0836 0.8521 0.032 Uiso 1 1 calc R U . . .
C23 C 0.7903(3) 0.0211(3) 0.88197(15) 0.0260(8) Uani 1 1 d . . . . .
H24 H 0.8122 0.0166 0.9226 0.031 Uiso 1 1 calc R U . . .
C24 C 0.7469(3) 0.0870(3) 0.86521(15) 0.0238(7) Uani 1 1 d . . . . .
C25 C 0.7197(3) 0.0963(3) 0.80609(15) 0.0254(8) Uani 1 1 d . . . . .
H25 H 0.6915 0.1420 0.7942 0.031 Uiso 1 1 calc R U . . .
C26 C 0.7335(3) 0.0387(3) 0.76415(15) 0.0260(8) Uani 1 1 d . . . . .
H26 H 0.7161 0.0468 0.7239 0.031 Uiso 1 1 calc R U . . .
P2 P 0.72897(7) 0.15975(7) 0.92145(4) 0.02208(19) Uani 1 1 d . . . . .
Pd2 Pd 0.61487(2) 0.23009(2) 0.88722(2) 0.02127(8) Uani 1 1 d . . . . .
P3 P 0.50239(7) 0.30314(7) 0.84940(4) 0.02080(18) Uani 1 1 d . . . . .
C27 C 0.3931(3) 0.2326(3) 0.78045(15) 0.0218(7) Uani 1 1 d . . . . .
C28 C 0.3097(3) 0.1371(3) 0.78226(15) 0.0228(7) Uani 1 1 d . . . . .
H27 H 0.3131 0.1117 0.8184 0.027 Uiso 1 1 calc R U . . .
C29 C 0.2233(3) 0.0798(3) 0.73250(15) 0.0233(7) Uani 1 1 d . . . . .
H28 H 0.1674 0.0158 0.7348 0.028 Uiso 1 1 calc R U . . .
C30 C 0.2166(3) 0.1147(3) 0.67831(14) 0.0219(7) Uani 1 1 d . . . . .
C31 C 0.2997(3) 0.2103(3) 0.67703(15) 0.0235(7) Uani 1 1 d . . . . .
H29 H 0.2965 0.2356 0.6408 0.028 Uiso 1 1 calc R U . . .
C32 C 0.3862(3) 0.2688(3) 0.72701(15) 0.0230(7) Uani 1 1 d . . . . .
H30 H 0.4410 0.3338 0.7250 0.028 Uiso 1 1 calc R U . . .
C33 C 0.1189(3) 0.0566(3) 0.62572(15) 0.0239(7) Uani 1 1 d . . . . .
C34 C 0.0717(3) 0.1144(3) 0.59895(15) 0.0284(8) Uani 1 1 d . . . . .
H51 H 0.1102 0.1875 0.6093 0.034 Uiso 1 1 calc R U . . .
C35 C -0.0312(3) 0.0671(3) 0.55708(16) 0.0341(9) Uani 1 1 d . . . . .
H52 H -0.0606 0.1078 0.5377 0.041 Uiso 1 1 calc R U . . .
C36 C -0.0885(3) -0.0373(3) 0.54439(16) 0.0329(9) Uani 1 1 d . . . . .
H53 H -0.1603 -0.0692 0.5181 0.039 Uiso 1 1 calc R U . . .
C37 C -0.0443(3) -0.0987(3) 0.56919(15) 0.0284(8) Uani 1 1 d . . . . .
C38 C -0.1100(3) -0.2085(3) 0.55822(17) 0.0364(9) Uani 1 1 d . . . . .
H54 H -0.1803 -0.2391 0.5303 0.044 Uiso 1 1 calc R U . . .
C39 C -0.0742(3) -0.2686(3) 0.58649(17) 0.0366(9) Uani 1 1 d . . . . .
H55 H -0.1225 -0.3398 0.5823 0.044 Uiso 1 1 calc R U . . .
C40 C 0.0359(3) -0.2275(3) 0.62302(16) 0.0310(8) Uani 1 1 d . . . . .
C41 C 0.0724(3) -0.2919(3) 0.65286(19) 0.0386(10) Uani 1 1 d . . . . .
H56 H 0.0229 -0.3620 0.6504 0.046 Uiso 1 1 calc R U . . .
C42 C 0.1781(3) -0.2541(3) 0.6851(2) 0.0419(10) Uani 1 1 d . . . . .
H57 H 0.2009 -0.2947 0.7092 0.050 Uiso 1 1 calc R U . . .
C43 C 0.2522(3) -0.1552(3) 0.68236(18) 0.0332(9) Uani 1 1 d . . . . .
H73 H 0.3265 -0.1310 0.7027 0.040 Uiso 1 1 calc R U . . .
C44 C 0.2212(3) -0.0914(3) 0.65107(15) 0.0238(7) Uani 1 1 d . . . . .
C45 C 0.1087(3) -0.1218(3) 0.62742(15) 0.0248(7) Uani 1 1 d . . . . .
C46 C 0.0640(3) -0.0531(3) 0.60722(14) 0.0242(7) Uani 1 1 d . . . . .
C47 C 0.3063(3) -0.0028(3) 0.63574(15) 0.0211(7) Uani 1 1 d . . . . .
C48 C 0.2868(3) 0.0163(3) 0.57775(15) 0.0228(7) Uani 1 1 d . . . . .
H58 H 0.2173 -0.0238 0.5497 0.027 Uiso 1 1 calc R U . . .
C49 C 0.3667(3) 0.0925(3) 0.56051(15) 0.0229(7) Uani 1 1 d . . . . .
H59 H 0.3509 0.1059 0.5213 0.027 Uiso 1 1 calc R U . . .
C50 C 0.4703(3) 0.1496(2) 0.60038(15) 0.0206(7) Uani 1 1 d . . . . .
C51 C 0.4909(3) 0.1297(3) 0.65793(15) 0.0223(7) Uani 1 1 d . . . . .
H60 H 0.5612 0.1679 0.6856 0.027 Uiso 1 1 calc R U . . .
C52 C 0.4093(3) 0.0544(3) 0.67517(15) 0.0236(7) Uani 1 1 d . . . . .
H61 H 0.4245 0.0421 0.7146 0.028 Uiso 1 1 calc R U . . .
P4 P 0.57473(7) 0.25793(6) 0.58254(4) 0.02051(18) Uani 1 1 d . . . . .
Cl1 Cl 0.79900(7) 0.47851(6) 0.64222(4) 0.0327(2) Uani 1 1 d . . . . .
Cl2 Cl 0.70414(7) 0.13578(6) 0.62334(4) 0.02697(19) Uani 1 1 d . . . . .
C53 C 1.0130(3) 0.3847(3) 0.64559(16) 0.0269(8) Uani 1 1 d . . . . .
C54 C 0.9717(4) 0.3935(4) 0.58786(19) 0.0464(11) Uani 1 1 d . . . . .
H13 H 0.9027 0.3902 0.5749 0.056 Uiso 1 1 calc R U . . .
C55 C 1.0310(4) 0.4071(4) 0.5487(2) 0.0627(14) Uani 1 1 d . . . . .
H14 H 1.0013 0.4110 0.5088 0.075 Uiso 1 1 calc R U . . .
C56 C 1.1325(4) 0.4149(4) 0.5673(2) 0.0515(12) Uani 1 1 d . . . . .
H15 H 1.1735 0.4259 0.5407 0.062 Uiso 1 1 calc R U . . .
C57 C 1.1739(3) 0.4066(3) 0.6249(2) 0.0377(10) Uani 1 1 d . . . . .
H16 H 1.2441 0.4126 0.6382 0.045 Uiso 1 1 calc R U . . .
C58 C 1.1144(3) 0.3898(3) 0.66349(18) 0.0322(8) Uani 1 1 d . . . . .
H17 H 1.1427 0.3816 0.7026 0.039 Uiso 1 1 calc R U . . .
C59 C 0.9875(3) 0.4605(3) 0.75592(15) 0.0247(7) Uani 1 1 d . . . . .
C60 C 1.0961(3) 0.5320(3) 0.77581(17) 0.0329(9) Uani 1 1 d . . . . .
H18 H 1.1414 0.5344 0.7529 0.039 Uiso 1 1 calc R U . . .
C61 C 1.1383(3) 0.6001(3) 0.8291(2) 0.0441(11) Uani 1 1 d . . . . .
H19 H 1.2127 0.6488 0.8426 0.053 Uiso 1 1 calc R U . . .
C62 C 1.0734(3) 0.5979(3) 0.86274(19) 0.0425(10) Uani 1 1 d . . . . .
H20 H 1.1035 0.6438 0.8997 0.051 Uiso 1 1 calc R U . . .
C63 C 0.9642(4) 0.5286(3) 0.84257(18) 0.0389(10) Uani 1 1 d . . . . .
H21 H 0.9189 0.5276 0.8652 0.047 Uiso 1 1 calc R U . . .
C64 C 0.9217(3) 0.4609(3) 0.78920(17) 0.0312(8) Uani 1 1 d . . . . .
H22 H 0.8467 0.4141 0.7750 0.037 Uiso 1 1 calc R U . . .
C65 C 0.8685(3) 0.2439(3) 0.96632(15) 0.0258(8) Uani 1 1 d . . . . .
C66 C 0.9197(3) 0.2153(3) 1.01494(16) 0.0320(8) Uani 1 1 d . . . . .
H31 H 0.8798 0.1536 1.0277 0.038 Uiso 1 1 calc R U . . .
C67 C 1.0288(3) 0.2767(3) 1.04489(18) 0.0388(10) Uani 1 1 d . . . . .
H32 H 1.0636 0.2568 1.0779 0.047 Uiso 1 1 calc R U . . .
C68 C 1.0867(3) 0.3667(3) 1.02655(18) 0.0401(10) Uani 1 1 d . . . . .
H33 H 1.1611 0.4093 1.0473 0.048 Uiso 1 1 calc R U . . .
C69 C 1.0363(3) 0.3950(3) 0.97784(19) 0.0416(10) Uani 1 1 d . . . . .
H34 H 1.0764 0.4565 0.9649 0.050 Uiso 1 1 calc R U . . .
C70 C 0.9277(3) 0.3337(3) 0.94802(17) 0.0351(9) Uani 1 1 d . . . . .
H35 H 0.8934 0.3534 0.9147 0.042 Uiso 1 1 calc R U . . .
C71 C 0.6714(3) 0.0707(3) 0.96810(15) 0.0262(8) Uani 1 1 d . . . . .
C72 C 0.6179(3) -0.0360(3) 0.94828(17) 0.0312(8) Uani 1 1 d . . . . .
H36 H 0.6131 -0.0635 0.9101 0.037 Uiso 1 1 calc R U . . .
C73 C 0.5720(3) -0.1013(3) 0.98423(19) 0.0388(9) Uani 1 1 d . . . . .
H37 H 0.5363 -0.1738 0.9709 0.047 Uiso 1 1 calc R U . . .
C74 C 0.5778(3) -0.0619(3) 1.03895(19) 0.0399(10) Uani 1 1 d . . . . .
H38 H 0.5471 -0.1075 1.0637 0.048 Uiso 1 1 calc R U . . .
C75 C 0.6277(3) 0.0430(4) 1.05869(17) 0.0389(10) Uani 1 1 d . . . . .
H39 H 0.6301 0.0694 1.0965 0.047 Uiso 1 1 calc R U . . .
C76 C 0.6747(3) 0.1102(3) 1.02303(16) 0.0321(8) Uani 1 1 d . . . . .
H40 H 0.7088 0.1827 1.0363 0.038 Uiso 1 1 calc R U . . .
Cl3 Cl 0.49813(7) 0.06997(6) 0.82929(4) 0.02560(18) Uani 1 1 d . . . . .
Cl4 Cl 0.72433(8) 0.37814(8) 0.95658(5) 0.0441(3) Uani 1 1 d . . . . .
C77 C 0.4326(3) 0.3287(3) 0.89659(15) 0.0258(8) Uani 1 1 d . . . . .
C78 C 0.3468(3) 0.3483(3) 0.87192(18) 0.0387(10) Uani 1 1 d . . . . .
H41 H 0.3227 0.3450 0.8303 0.046 Uiso 1 1 calc R U . . .
C79 C 0.2965(3) 0.3725(4) 0.9078(2) 0.0480(11) Uani 1 1 d . . . . .
H42 H 0.2383 0.3862 0.8908 0.058 Uiso 1 1 calc R U . . .
C80 C 0.3311(4) 0.3765(4) 0.9681(2) 0.0529(12) Uani 1 1 d . . . . .
H43 H 0.2960 0.3920 0.9927 0.063 Uiso 1 1 calc R U . . .
C81 C 0.4162(4) 0.3584(4) 0.9927(2) 0.0567(13) Uani 1 1 d . . . . .
H44 H 0.4403 0.3621 1.0343 0.068 Uiso 1 1 calc R U . . .
C82 C 0.4676(4) 0.3344(3) 0.95704(17) 0.0384(9) Uani 1 1 d . . . . .
H45 H 0.5267 0.3221 0.9744 0.046 Uiso 1 1 calc R U . . .
C83 C 0.5855(3) 0.4298(3) 0.83450(14) 0.0228(7) Uani 1 1 d . . . . .
C84 C 0.5952(3) 0.5188(3) 0.86215(16) 0.0303(8) Uani 1 1 d . . . . .
H46 H 0.5540 0.5152 0.8879 0.036 Uiso 1 1 calc R U . . .
C85 C 0.6647(3) 0.6141(3) 0.85288(17) 0.0355(9) Uani 1 1 d . . . . .
H47 H 0.6723 0.6752 0.8733 0.043 Uiso 1 1 calc R U . . .
C86 C 0.7226(3) 0.6208(3) 0.81438(17) 0.0350(9) Uani 1 1 d . . . . .
H48 H 0.7678 0.6861 0.8070 0.042 Uiso 1 1 calc R U . . .
C87 C 0.7145(3) 0.5320(3) 0.78667(17) 0.0327(9) Uani 1 1 d . . . . .
H49 H 0.7545 0.5359 0.7602 0.039 Uiso 1 1 calc R U . . .
C88 C 0.6478(3) 0.4371(3) 0.79743(16) 0.0305(8) Uani 1 1 d . . . . .
H50 H 0.6444 0.3763 0.7794 0.037 Uiso 1 1 calc R U . . .
C89 C 0.5726(3) 0.2287(3) 0.50733(15) 0.0237(7) Uani 1 1 d . . . . .
C90 C 0.6372(3) 0.3119(3) 0.48482(16) 0.0294(8) Uani 1 1 d . . . . .
H62 H 0.6738 0.3797 0.5075 0.035 Uiso 1 1 calc R U . . .
C91 C 0.6475(3) 0.2954(3) 0.43002(18) 0.0368(9) Uani 1 1 d . . . . .
H63 H 0.6913 0.3517 0.4148 0.044 Uiso 1 1 calc R U . . .
C92 C 0.5941(3) 0.1969(3) 0.39712(18) 0.0401(10) Uani 1 1 d . . . . .
H64 H 0.5995 0.1859 0.3587 0.048 Uiso 1 1 calc R U . . .
C93 C 0.5329(3) 0.1140(3) 0.41962(17) 0.0325(9) Uani 1 1 d . . . . .
H65 H 0.4987 0.0462 0.3972 0.039 Uiso 1 1 calc R U . . .
C94 C 0.5211(3) 0.1291(3) 0.47429(16) 0.0278(8) Uani 1 1 d . . . . .
H66 H 0.4783 0.0721 0.4894 0.033 Uiso 1 1 calc R U . . .
C95 C 0.5222(3) 0.3507(3) 0.58047(15) 0.0232(7) Uani 1 1 d . . . . .
C96 C 0.4522(3) 0.3534(3) 0.52884(16) 0.0289(8) Uani 1 1 d . . . . .
H67 H 0.4359 0.3111 0.4925 0.035 Uiso 1 1 calc R U . . .
C97 C 0.4061(3) 0.4182(3) 0.53056(19) 0.0355(9) Uani 1 1 d . . . . .
H68 H 0.3579 0.4201 0.4955 0.043 Uiso 1 1 calc R U . . .
C98 C 0.4308(3) 0.4798(3) 0.5835(2) 0.0380(10) Uani 1 1 d . . . . .
H69 H 0.3999 0.5244 0.5846 0.046 Uiso 1 1 calc R U . . .
C99 C 0.4996(3) 0.4770(3) 0.63465(19) 0.0354(9) Uani 1 1 d . . . . .
H70 H 0.5161 0.5195 0.6709 0.042 Uiso 1 1 calc R U . . .
C100 C 0.5447(3) 0.4122(3) 0.63323(17) 0.0292(8) Uani 1 1 d . . . . .
H71 H 0.5915 0.4098 0.6687 0.035 Uiso 1 1 calc R U . . .
C101 C 1.4768(4) 0.7094(4) 0.7863(2) 0.0586(13) Uani 1 1 d . . . . .
H72 H 1.5492 0.7146 0.7906 0.070 Uiso 1 1 calc R U . . .
Cl5 Cl 1.43493(14) 0.65777(14) 0.84665(7) 0.0840(5) Uani 1 1 d . . . . .
Cl6 Cl 1.48865(11) 0.83221(10) 0.78700(6) 0.0646(3) Uani 1 1 d . . . . .
Cl7 Cl 1.38591(14) 0.62573(12) 0.72004(7) 0.0839(5) Uani 1 1 d . . . . .
O1 O 0.8279(6) -0.1392(7) 0.9882(4) 0.079(2) Uani 0.5 1 d D U P A -1
H74 H 0.8153 -0.1717 0.9548 0.119 Uiso 0.5 1 calc R U P A -1
C102 C 0.9373(8) -0.0577(11) 1.0081(8) 0.121(4) Uani 0.5 1 d D U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.2904(9) . ?
Pd1 Cl2 2.2906(8) . ?
Pd1 P4 2.3204(9) . ?
Pd1 P1 2.3341(9) . ?
P1 C1 1.821(3) . ?
P1 C59 1.822(3) . ?
P1 C53 1.826(4) . ?
C1 C6 1.391(5) . ?
C1 C2 1.397(5) . ?
C2 C3 1.380(5) . ?
C3 C4 1.399(5) . ?
C4 C5 1.401(5) . ?
C4 C7 1.490(5) . ?
C5 C6 1.379(5) . ?
C7 C8 1.384(5) . ?
C7 C20 1.429(5) . ?
C8 C9 1.384(6) . ?
C9 C10 1.365(6) . ?
C10 C11 1.411(6) . ?
C11 C20 1.419(5) . ?
C11 C12 1.419(6) . ?
C12 C13 1.329(7) . ?
C13 C14 1.441(6) . ?
C14 C15 1.405(6) . ?
C14 C19 1.420(5) . ?
C15 C16 1.353(7) . ?
C16 C17 1.398(6) . ?
C17 C18 1.390(5) . ?
C18 C19 1.426(5) . ?
C18 C21 1.486(5) . ?
C19 C20 1.457(5) . ?
C21 C26 1.388(5) . ?
C21 C22 1.402(5) . ?
C22 C23 1.379(5) . ?
C23 C24 1.395(5) . ?
C24 C25 1.387(5) . ?
C24 P2 1.818(3) . ?
C25 C26 1.390(5) . ?
P2 C71 1.814(4) . ?
P2 C65 1.823(4) . ?
P2 Pd2 2.3216(9) . ?
Pd2 Cl4 2.2887(10) . ?
Pd2 Cl3 2.2978(9) . ?
Pd2 P3 2.3511(9) . ?
P3 C27 1.822(3) . ?
P3 C77 1.825(3) . ?
P3 C83 1.829(3) . ?
C27 C32 1.395(5) . ?
C27 C28 1.405(5) . ?
C28 C29 1.374(5) . ?
C29 C30 1.403(5) . ?
C30 C31 1.400(5) . ?
C30 C33 1.489(5) . ?
C31 C32 1.381(5) . ?
C33 C34 1.392(5) . ?
C33 C46 1.431(5) . ?
C34 C35 1.399(5) . ?
C35 C36 1.356(6) . ?
C36 C37 1.395(5) . ?
C37 C46 1.422(5) . ?
C37 C38 1.433(5) . ?
C38 C39 1.336(6) . ?
C39 C40 1.435(5) . ?
C40 C41 1.411(6) . ?
C40 C45 1.422(5) . ?
C41 C42 1.362(6) . ?
C42 C43 1.394(5) . ?
C43 C44 1.379(5) . ?
C44 C45 1.432(5) . ?
C44 C47 1.488(5) . ?
C45 C46 1.463(5) . ?
C47 C52 1.383(5) . ?
C47 C48 1.399(5) . ?
C48 C49 1.383(5) . ?
C49 C50 1.393(5) . ?
C50 C51 1.394(5) . ?
C50 P4 1.812(3) . ?
C51 C52 1.392(5) . ?
P4 C89 1.808(4) . ?
P4 C95 1.834(3) . ?
C53 C54 1.383(5) . ?
C53 C58 1.394(5) . ?
C54 C55 1.392(6) . ?
C55 C56 1.378(7) . ?
C56 C57 1.380(6) . ?
C57 C58 1.377(5) . ?
C59 C60 1.387(5) . ?
C59 C64 1.394(5) . ?
C60 C61 1.385(6) . ?
C61 C62 1.380(6) . ?
C62 C63 1.386(6) . ?
C63 C64 1.384(5) . ?
C65 C70 1.384(5) . ?
C65 C66 1.392(5) . ?
C66 C67 1.390(5) . ?
C67 C68 1.381(6) . ?
C68 C69 1.386(6) . ?
C69 C70 1.384(6) . ?
C71 C76 1.386(5) . ?
C71 C72 1.397(5) . ?
C72 C73 1.378(5) . ?
C73 C74 1.366(6) . ?
C74 C75 1.377(6) . ?
C75 C76 1.394(5) . ?
C77 C82 1.378(5) . ?
C77 C78 1.393(5) . ?
C78 C79 1.385(6) . ?
C79 C80 1.380(7) . ?
C80 C81 1.371(7) . ?
C81 C82 1.393(6) . ?
C83 C84 1.371(5) . ?
C83 C88 1.396(5) . ?
C84 C85 1.387(5) . ?
C85 C86 1.377(5) . ?
C86 C87 1.379(5) . ?
C87 C88 1.384(5) . ?
C89 C94 1.394(5) . ?
C89 C90 1.404(5) . ?
C90 C91 1.372(5) . ?
C91 C92 1.378(6) . ?
C92 C93 1.383(5) . ?
C93 C94 1.375(5) . ?
C95 C100 1.386(5) . ?
C95 C96 1.390(5) . ?
C96 C97 1.394(5) . ?
C97 C98 1.381(6) . ?
C98 C99 1.374(6) . ?
C99 C100 1.380(5) . ?
C101 Cl6 1.736(5) . ?
C101 Cl7 1.745(5) . ?
C101 Cl5 1.774(5) . ?
O1 C102 1.436(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl2 170.76(4) . . ?
Cl1 Pd1 P4 91.99(3) . . ?
Cl2 Pd1 P4 86.21(3) . . ?
Cl1 Pd1 P1 88.96(3) . . ?
Cl2 Pd1 P1 92.39(3) . . ?
P4 Pd1 P1 176.93(3) . . ?
C1 P1 C59 101.34(16) . . ?
C1 P1 C53 103.01(16) . . ?
C59 P1 C53 109.43(16) . . ?
C1 P1 Pd1 117.59(11) . . ?
C59 P1 Pd1 113.59(11) . . ?
C53 P1 Pd1 110.96(12) . . ?
C6 C1 C2 118.9(3) . . ?
C6 C1 P1 122.5(3) . . ?
C2 C1 P1 118.6(3) . . ?
C3 C2 C1 120.4(3) . . ?
C2 C3 C4 120.9(3) . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C7 120.5(3) . . ?
C5 C4 C7 120.9(3) . . ?
C6 C5 C4 120.6(3) . . ?
C5 C6 C1 120.8(3) . . ?
C8 C7 C20 119.4(3) . . ?
C8 C7 C4 117.0(3) . . ?
C20 C7 C4 123.0(3) . . ?
C9 C8 C7 122.4(4) . . ?
C10 C9 C8 118.4(4) . . ?
C9 C10 C11 121.6(4) . . ?
C10 C11 C20 119.7(4) . . ?
C10 C11 C12 120.4(4) . . ?
C20 C11 C12 119.8(4) . . ?
C13 C12 C11 120.9(4) . . ?
C12 C13 C14 121.4(4) . . ?
C15 C14 C19 120.7(4) . . ?
C15 C14 C13 120.2(4) . . ?
C19 C14 C13 118.9(4) . . ?
C16 C15 C14 120.7(4) . . ?
C15 C16 C17 119.6(4) . . ?
C18 C17 C16 121.5(4) . . ?
C17 C18 C19 119.4(3) . . ?
C17 C18 C21 115.5(3) . . ?
C19 C18 C21 124.4(3) . . ?
C14 C19 C18 117.0(4) . . ?
C14 C19 C20 117.8(3) . . ?
C18 C19 C20 125.1(3) . . ?
C11 C20 C7 116.9(3) . . ?
C11 C20 C19 117.9(3) . . ?
C7 C20 C19 125.2(3) . . ?
C26 C21 C22 118.6(3) . . ?
C26 C21 C18 121.6(3) . . ?
C22 C21 C18 119.5(3) . . ?
C23 C22 C21 120.4(3) . . ?
C22 C23 C24 120.8(3) . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 P2 121.6(3) . . ?
C23 C24 P2 119.3(3) . . ?
C24 C25 C26 120.1(3) . . ?
C21 C26 C25 121.0(3) . . ?
C71 P2 C24 106.47(16) . . ?
C71 P2 C65 105.06(16) . . ?
C24 P2 C65 101.13(16) . . ?
C71 P2 Pd2 107.13(11) . . ?
C24 P2 Pd2 116.25(12) . . ?
C65 P2 Pd2 119.66(12) . . ?
Cl4 Pd2 Cl3 171.38(4) . . ?
Cl4 Pd2 P2 92.10(3) . . ?
Cl3 Pd2 P2 85.40(3) . . ?
Cl4 Pd2 P3 88.31(3) . . ?
Cl3 Pd2 P3 94.52(3) . . ?
P2 Pd2 P3 177.66(3) . . ?
C27 P3 C77 102.18(16) . . ?
C27 P3 C83 106.06(15) . . ?
C77 P3 C83 104.26(16) . . ?
C27 P3 Pd2 116.81(11) . . ?
C77 P3 Pd2 118.16(12) . . ?
C83 P3 Pd2 108.12(11) . . ?
C32 C27 C28 118.6(3) . . ?
C32 C27 P3 124.2(3) . . ?
C28 C27 P3 117.2(3) . . ?
C29 C28 C27 121.0(3) . . ?
C28 C29 C30 120.9(3) . . ?
C31 C30 C29 117.7(3) . . ?
C31 C30 C33 121.3(3) . . ?
C29 C30 C33 120.7(3) . . ?
C32 C31 C30 121.7(3) . . ?
C31 C32 C27 120.1(3) . . ?
C34 C33 C46 119.3(3) . . ?
C34 C33 C30 115.2(3) . . ?
C46 C33 C30 124.8(3) . . ?
C33 C34 C35 121.4(4) . . ?
C36 C35 C34 119.4(4) . . ?
C35 C36 C37 121.3(3) . . ?
C36 C37 C46 120.5(3) . . ?
C36 C37 C38 119.7(3) . . ?
C46 C37 C38 119.7(3) . . ?
C39 C38 C37 121.3(3) . . ?
C38 C39 C40 121.1(3) . . ?
C41 C40 C45 120.3(3) . . ?
C41 C40 C39 120.5(3) . . ?
C45 C40 C39 119.2(3) . . ?
C42 C41 C40 120.5(3) . . ?
C41 C42 C43 119.2(4) . . ?
C44 C43 C42 122.1(4) . . ?
C43 C44 C45 118.9(3) . . ?
C43 C44 C47 117.1(3) . . ?
C45 C44 C47 123.2(3) . . ?
C40 C45 C44 116.6(3) . . ?
C40 C45 C46 118.3(3) . . ?
C44 C45 C46 125.1(3) . . ?
C37 C46 C33 117.2(3) . . ?
C37 C46 C45 117.8(3) . . ?
C33 C46 C45 124.9(3) . . ?
C52 C47 C48 118.2(3) . . ?
C52 C47 C44 121.8(3) . . ?
C48 C47 C44 119.6(3) . . ?
C49 C48 C47 121.3(3) . . ?
C48 C49 C50 120.2(3) . . ?
C49 C50 C51 118.8(3) . . ?
C49 C50 P4 122.1(3) . . ?
C51 C50 P4 118.8(2) . . ?
C52 C51 C50 120.5(3) . . ?
C47 C52 C51 121.0(3) . . ?
C89 P4 C50 110.71(16) . . ?
C89 P4 C95 104.92(16) . . ?
C50 P4 C95 100.70(15) . . ?
C89 P4 Pd1 104.62(11) . . ?
C50 P4 Pd1 115.73(11) . . ?
C95 P4 Pd1 119.71(11) . . ?
C54 C53 C58 118.8(3) . . ?
C54 C53 P1 119.4(3) . . ?
C58 C53 P1 121.5(3) . . ?
C53 C54 C55 120.1(4) . . ?
C56 C55 C54 120.6(4) . . ?
C55 C56 C57 119.2(4) . . ?
C58 C57 C56 120.6(4) . . ?
C57 C58 C53 120.5(4) . . ?
C60 C59 C64 119.0(3) . . ?
C60 C59 P1 123.5(3) . . ?
C64 C59 P1 116.9(3) . . ?
C61 C60 C59 119.9(4) . . ?
C62 C61 C60 120.8(4) . . ?
C61 C62 C63 119.9(4) . . ?
C64 C63 C62 119.5(4) . . ?
C63 C64 C59 120.9(4) . . ?
C70 C65 C66 119.2(3) . . ?
C70 C65 P2 118.8(3) . . ?
C66 C65 P2 121.7(3) . . ?
C67 C66 C65 120.3(4) . . ?
C68 C67 C66 119.9(4) . . ?
C67 C68 C69 120.1(4) . . ?
C70 C69 C68 120.0(4) . . ?
C69 C70 C65 120.6(4) . . ?
C76 C71 C72 119.6(3) . . ?
C76 C71 P2 118.7(3) . . ?
C72 C71 P2 121.6(3) . . ?
C73 C72 C71 119.9(4) . . ?
C74 C73 C72 120.2(4) . . ?
C73 C74 C75 120.8(4) . . ?
C74 C75 C76 119.9(4) . . ?
C71 C76 C75 119.5(4) . . ?
C82 C77 C78 119.4(3) . . ?
C82 C77 P3 120.6(3) . . ?
C78 C77 P3 119.9(3) . . ?
C79 C78 C77 120.3(4) . . ?
C80 C79 C78 119.8(4) . . ?
C81 C80 C79 120.1(4) . . ?
C80 C81 C82 120.6(4) . . ?
C77 C82 C81 119.8(4) . . ?
C84 C83 C88 118.7(3) . . ?
C84 C83 P3 122.1(3) . . ?
C88 C83 P3 119.0(3) . . ?
C83 C84 C85 120.5(3) . . ?
C86 C85 C84 120.6(4) . . ?
C85 C86 C87 119.5(4) . . ?
C86 C87 C88 119.9(3) . . ?
C87 C88 C83 120.8(3) . . ?
C94 C89 C90 119.6(3) . . ?
C94 C89 P4 123.9(3) . . ?
C90 C89 P4 116.1(3) . . ?
C91 C90 C89 120.0(3) . . ?
C90 C91 C92 119.9(3) . . ?
C91 C92 C93 120.6(4) . . ?
C94 C93 C92 120.4(3) . . ?
C93 C94 C89 119.5(3) . . ?
C100 C95 C96 119.4(3) . . ?
C100 C95 P4 118.5(3) . . ?
C96 C95 P4 121.7(3) . . ?
C95 C96 C97 119.8(4) . . ?
C98 C97 C96 119.7(4) . . ?
C99 C98 C97 120.6(4) . . ?
C98 C99 C100 119.8(4) . . ?
C99 C100 C95 120.6(4) . . ?
Cl6 C101 Cl7 111.8(3) . . ?
Cl6 C101 Cl5 110.6(3) . . ?
Cl7 C101 Cl5 109.3(3) . . ?

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
C59 P1 C1 C6 17.3(3) . . . . ?
C53 P1 C1 C6 130.5(3) . . . . ?
Pd1 P1 C1 C6 -107.1(3) . . . . ?
C59 P1 C1 C2 -163.1(3) . . . . ?
C53 P1 C1 C2 -49.8(3) . . . . ?
Pd1 P1 C1 C2 72.5(3) . . . . ?
C6 C1 C2 C3 -0.1(5) . . . . ?
P1 C1 C2 C3 -179.8(2) . . . . ?
C1 C2 C3 C4 1.0(5) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C7 -175.6(3) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C7 C4 C5 C6 174.8(3) . . . . ?
C4 C5 C6 C1 0.6(5) . . . . ?
C2 C1 C6 C5 -0.6(5) . . . . ?
P1 C1 C6 C5 179.0(3) . . . . ?
C3 C4 C7 C8 130.1(4) . . . . ?
C5 C4 C7 C8 -44.4(5) . . . . ?
C3 C4 C7 C20 -40.8(5) . . . . ?
C5 C4 C7 C20 144.7(3) . . . . ?
C20 C7 C8 C9 3.8(6) . . . . ?
C4 C7 C8 C9 -167.5(4) . . . . ?
C7 C8 C9 C10 6.2(6) . . . . ?
C8 C9 C10 C11 -6.8(6) . . . . ?
C9 C10 C11 C20 -2.7(6) . . . . ?
C9 C10 C11 C12 173.6(4) . . . . ?
C10 C11 C12 C13 -175.0(4) . . . . ?
C20 C11 C12 C13 1.2(6) . . . . ?
C11 C12 C13 C14 -10.0(6) . . . . ?
C12 C13 C14 C15 -172.2(4) . . . . ?
C12 C13 C14 C19 3.0(6) . . . . ?
C19 C14 C15 C16 -2.9(6) . . . . ?
C13 C14 C15 C16 172.2(4) . . . . ?
C14 C15 C16 C17 -4.8(6) . . . . ?
C15 C16 C17 C18 4.2(6) . . . . ?
C16 C17 C18 C19 4.2(6) . . . . ?
C16 C17 C18 C21 -166.8(4) . . . . ?
C15 C14 C19 C18 10.9(5) . . . . ?
C13 C14 C19 C18 -164.2(3) . . . . ?
C15 C14 C19 C20 -172.6(3) . . . . ?
C13 C14 C19 C20 12.3(5) . . . . ?
C17 C18 C19 C14 -11.4(5) . . . . ?
C21 C18 C19 C14 158.7(3) . . . . ?
C17 C18 C19 C20 172.3(3) . . . . ?
C21 C18 C19 C20 -17.6(5) . . . . ?
C10 C11 C20 C7 12.3(5) . . . . ?
C12 C11 C20 C7 -163.9(3) . . . . ?
C10 C11 C20 C19 -169.7(3) . . . . ?
C12 C11 C20 C19 14.0(5) . . . . ?
C8 C7 C20 C11 -12.8(5) . . . . ?
C4 C7 C20 C11 157.9(3) . . . . ?
C8 C7 C20 C19 169.4(3) . . . . ?
C4 C7 C20 C19 -19.9(5) . . . . ?
C14 C19 C20 C11 -20.4(5) . . . . ?
C18 C19 C20 C11 155.8(3) . . . . ?
C14 C19 C20 C7 157.3(3) . . . . ?
C18 C19 C20 C7 -26.4(5) . . . . ?
C17 C18 C21 C26 -44.7(5) . . . . ?
C19 C18 C21 C26 144.9(3) . . . . ?
C17 C18 C21 C22 129.1(4) . . . . ?
C19 C18 C21 C22 -41.3(5) . . . . ?
C26 C21 C22 C23 1.1(5) . . . . ?
C18 C21 C22 C23 -172.9(3) . . . . ?
C21 C22 C23 C24 1.6(5) . . . . ?
C22 C23 C24 C25 -2.9(5) . . . . ?
C22 C23 C24 P2 177.9(3) . . . . ?
C23 C24 C25 C26 1.4(5) . . . . ?
P2 C24 C25 C26 -179.4(3) . . . . ?
C22 C21 C26 C25 -2.6(5) . . . . ?
C18 C21 C26 C25 171.2(3) . . . . ?
C24 C25 C26 C21 1.4(5) . . . . ?
C25 C24 P2 C71 136.5(3) . . . . ?
C23 C24 P2 C71 -44.3(3) . . . . ?
C25 C24 P2 C65 -114.0(3) . . . . ?
C23 C24 P2 C65 65.2(3) . . . . ?
C25 C24 P2 Pd2 17.3(3) . . . . ?
C23 C24 P2 Pd2 -163.5(2) . . . . ?
C77 P3 C27 C32 115.1(3) . . . . ?
C83 P3 C27 C32 6.2(3) . . . . ?
Pd2 P3 C27 C32 -114.3(3) . . . . ?
C77 P3 C27 C28 -63.1(3) . . . . ?
C83 P3 C27 C28 -172.1(3) . . . . ?
Pd2 P3 C27 C28 67.4(3) . . . . ?
C32 C27 C28 C29 0.5(5) . . . . ?
P3 C27 C28 C29 178.8(3) . . . . ?
C27 C28 C29 C30 0.7(5) . . . . ?
C28 C29 C30 C31 -1.1(5) . . . . ?
C28 C29 C30 C33 -175.2(3) . . . . ?
C29 C30 C31 C32 0.4(5) . . . . ?
C33 C30 C31 C32 174.4(3) . . . . ?
C30 C31 C32 C27 0.8(5) . . . . ?
C28 C27 C32 C31 -1.2(5) . . . . ?
P3 C27 C32 C31 -179.4(2) . . . . ?
C31 C30 C33 C34 -47.2(4) . . . . ?
C29 C30 C33 C34 126.6(3) . . . . ?
C31 C30 C33 C46 142.1(3) . . . . ?
C29 C30 C33 C46 -44.0(5) . . . . ?
C46 C33 C34 C35 4.1(5) . . . . ?
C30 C33 C34 C35 -167.1(3) . . . . ?
C33 C34 C35 C36 3.3(5) . . . . ?
C34 C35 C36 C37 -4.4(6) . . . . ?
C35 C36 C37 C46 -2.0(5) . . . . ?
C35 C36 C37 C38 175.4(4) . . . . ?
C36 C37 C38 C39 -172.3(4) . . . . ?
C46 C37 C38 C39 5.1(6) . . . . ?
C37 C38 C39 C40 -8.3(6) . . . . ?
C38 C39 C40 C41 179.7(4) . . . . ?
C38 C39 C40 C45 -2.2(6) . . . . ?
C45 C40 C41 C42 -1.4(6) . . . . ?
C39 C40 C41 C42 176.7(4) . . . . ?
C40 C41 C42 C43 -8.0(6) . . . . ?
C41 C42 C43 C44 4.4(6) . . . . ?
C42 C43 C44 C45 8.6(6) . . . . ?
C42 C43 C44 C47 -161.9(4) . . . . ?
C41 C40 C45 C44 14.0(5) . . . . ?
C39 C40 C45 C44 -164.2(3) . . . . ?
C41 C40 C45 C46 -166.6(3) . . . . ?
C39 C40 C45 C46 15.2(5) . . . . ?
C43 C44 C45 C40 -17.4(5) . . . . ?
C47 C44 C45 C40 152.5(3) . . . . ?
C43 C44 C45 C46 163.3(3) . . . . ?
C47 C44 C45 C46 -26.8(5) . . . . ?
C36 C37 C46 C33 9.2(5) . . . . ?
C38 C37 C46 C33 -168.2(3) . . . . ?
C36 C37 C46 C45 -174.5(3) . . . . ?
C38 C37 C46 C45 8.1(5) . . . . ?
C34 C33 C46 C37 -10.1(5) . . . . ?
C30 C33 C46 C37 160.2(3) . . . . ?
C34 C33 C46 C45 173.9(3) . . . . ?
C30 C33 C46 C45 -15.8(5) . . . . ?
C40 C45 C46 C37 -17.9(5) . . . . ?
C44 C45 C46 C37 161.4(3) . . . . ?
C40 C45 C46 C33 158.0(3) . . . . ?
C44 C45 C46 C33 -22.6(5) . . . . ?
C43 C44 C47 C52 -39.8(5) . . . . ?
C45 C44 C47 C52 150.1(3) . . . . ?
C43 C44 C47 C48 132.3(4) . . . . ?
C45 C44 C47 C48 -37.7(5) . . . . ?
C52 C47 C48 C49 -2.2(5) . . . . ?
C44 C47 C48 C49 -174.6(3) . . . . ?
C47 C48 C49 C50 2.4(5) . . . . ?
C48 C49 C50 C51 -1.2(5) . . . . ?
C48 C49 C50 P4 -174.2(3) . . . . ?
C49 C50 C51 C52 -0.2(5) . . . . ?
P4 C50 C51 C52 173.1(3) . . . . ?
C48 C47 C52 C51 0.8(5) . . . . ?
C44 C47 C52 C51 173.0(3) . . . . ?
C50 C51 C52 C47 0.4(5) . . . . ?
C49 C50 P4 C89 -42.1(3) . . . . ?
C51 C50 P4 C89 144.8(3) . . . . ?
C49 C50 P4 C95 68.5(3) . . . . ?
C51 C50 P4 C95 -104.6(3) . . . . ?
C49 C50 P4 Pd1 -160.9(2) . . . . ?
C51 C50 P4 Pd1 26.0(3) . . . . ?
C1 P1 C53 C54 136.2(3) . . . . ?
C59 P1 C53 C54 -116.6(3) . . . . ?
Pd1 P1 C53 C54 9.5(4) . . . . ?
C1 P1 C53 C58 -37.3(3) . . . . ?
C59 P1 C53 C58 69.9(3) . . . . ?
Pd1 P1 C53 C58 -164.0(3) . . . . ?
C58 C53 C54 C55 0.0(7) . . . . ?
P1 C53 C54 C55 -173.7(4) . . . . ?
C53 C54 C55 C56 -1.9(8) . . . . ?
C54 C55 C56 C57 1.6(8) . . . . ?
C55 C56 C57 C58 0.6(7) . . . . ?
C56 C57 C58 C53 -2.4(6) . . . . ?
C54 C53 C58 C57 2.1(6) . . . . ?
P1 C53 C58 C57 175.6(3) . . . . ?
C1 P1 C59 C60 84.8(3) . . . . ?
C53 P1 C59 C60 -23.5(4) . . . . ?
Pd1 P1 C59 C60 -148.1(3) . . . . ?
C1 P1 C59 C64 -86.5(3) . . . . ?
C53 P1 C59 C64 165.2(3) . . . . ?
Pd1 P1 C59 C64 40.5(3) . . . . ?
C64 C59 C60 C61 2.2(6) . . . . ?
P1 C59 C60 C61 -168.9(3) . . . . ?
C59 C60 C61 C62 -0.2(6) . . . . ?
C60 C61 C62 C63 -1.5(7) . . . . ?
C61 C62 C63 C64 1.2(6) . . . . ?
C62 C63 C64 C59 0.9(6) . . . . ?
C60 C59 C64 C63 -2.6(5) . . . . ?
P1 C59 C64 C63 169.1(3) . . . . ?
C71 P2 C65 C70 -166.5(3) . . . . ?
C24 P2 C65 C70 82.9(3) . . . . ?
Pd2 P2 C65 C70 -46.2(3) . . . . ?
C71 P2 C65 C66 19.9(3) . . . . ?
C24 P2 C65 C66 -90.8(3) . . . . ?
Pd2 P2 C65 C66 140.1(3) . . . . ?
C70 C65 C66 C67 0.4(6) . . . . ?
P2 C65 C66 C67 174.0(3) . . . . ?
C65 C66 C67 C68 0.3(6) . . . . ?
C66 C67 C68 C69 -0.9(6) . . . . ?
C67 C68 C69 C70 0.8(6) . . . . ?
C68 C69 C70 C65 -0.1(6) . . . . ?
C66 C65 C70 C69 -0.5(6) . . . . ?
P2 C65 C70 C69 -174.3(3) . . . . ?
C24 P2 C71 C76 163.6(3) . . . . ?
C65 P2 C71 C76 56.9(3) . . . . ?
Pd2 P2 C71 C76 -71.4(3) . . . . ?
C24 P2 C71 C72 -20.8(3) . . . . ?
C65 P2 C71 C72 -127.5(3) . . . . ?
Pd2 P2 C71 C72 104.2(3) . . . . ?
C76 C71 C72 C73 -2.3(5) . . . . ?
P2 C71 C72 C73 -177.8(3) . . . . ?
C71 C72 C73 C74 0.7(6) . . . . ?
C72 C73 C74 C75 1.1(6) . . . . ?
C73 C74 C75 C76 -1.2(6) . . . . ?
C72 C71 C76 C75 2.2(5) . . . . ?
P2 C71 C76 C75 177.9(3) . . . . ?
C74 C75 C76 C71 -0.5(6) . . . . ?
C27 P3 C77 C82 148.5(3) . . . . ?
C83 P3 C77 C82 -101.2(3) . . . . ?
Pd2 P3 C77 C82 18.8(4) . . . . ?
C27 P3 C77 C78 -35.0(3) . . . . ?
C83 P3 C77 C78 75.3(3) . . . . ?
Pd2 P3 C77 C78 -164.7(3) . . . . ?
C82 C77 C78 C79 -0.5(6) . . . . ?
P3 C77 C78 C79 -177.0(3) . . . . ?
C77 C78 C79 C80 -0.4(7) . . . . ?
C78 C79 C80 C81 1.0(7) . . . . ?
C79 C80 C81 C82 -0.8(8) . . . . ?
C78 C77 C82 C81 0.8(6) . . . . ?
P3 C77 C82 C81 177.3(3) . . . . ?
C80 C81 C82 C77 -0.1(7) . . . . ?
C27 P3 C83 C84 114.6(3) . . . . ?
C77 P3 C83 C84 7.2(3) . . . . ?
Pd2 P3 C83 C84 -119.4(3) . . . . ?
C27 P3 C83 C88 -70.6(3) . . . . ?
C77 P3 C83 C88 -178.0(3) . . . . ?
Pd2 P3 C83 C88 55.4(3) . . . . ?
C88 C83 C84 C85 0.7(5) . . . . ?
P3 C83 C84 C85 175.6(3) . . . . ?
C83 C84 C85 C86 2.0(6) . . . . ?
C84 C85 C86 C87 -2.6(6) . . . . ?
C85 C86 C87 C88 0.4(6) . . . . ?
C86 C87 C88 C83 2.3(6) . . . . ?
C84 C83 C88 C87 -2.9(5) . . . . ?
P3 C83 C88 C87 -177.8(3) . . . . ?
C50 P4 C89 C94 -17.5(3) . . . . ?
C95 P4 C89 C94 -125.4(3) . . . . ?
Pd1 P4 C89 C94 107.8(3) . . . . ?
C50 P4 C89 C90 169.6(3) . . . . ?
C95 P4 C89 C90 61.8(3) . . . . ?
Pd1 P4 C89 C90 -65.0(3) . . . . ?
C94 C89 C90 C91 1.5(5) . . . . ?
P4 C89 C90 C91 174.6(3) . . . . ?
C89 C90 C91 C92 0.1(6) . . . . ?
C90 C91 C92 C93 -2.0(6) . . . . ?
C91 C92 C93 C94 2.4(6) . . . . ?
C92 C93 C94 C89 -0.8(6) . . . . ?
C90 C89 C94 C93 -1.1(5) . . . . ?
P4 C89 C94 C93 -173.7(3) . . . . ?
C89 P4 C95 C100 -159.9(3) . . . . ?
C50 P4 C95 C100 85.1(3) . . . . ?
Pd1 P4 C95 C100 -43.0(3) . . . . ?
C89 P4 C95 C96 26.6(3) . . . . ?
C50 P4 C95 C96 -88.4(3) . . . . ?
Pd1 P4 C95 C96 143.5(2) . . . . ?
C100 C95 C96 C97 0.4(5) . . . . ?
P4 C95 C96 C97 173.8(3) . . . . ?
C95 C96 C97 C98 0.4(5) . . . . ?
C96 C97 C98 C99 -0.6(6) . . . . ?
C97 C98 C99 C100 0.0(6) . . . . ?
C98 C99 C100 C95 0.8(5) . . . . ?
C96 C95 C100 C99 -1.0(5) . . . . ?
P4 C95 C100 C99 -174.6(3) . . . . ?

_refine_diff_density_max         2.383
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.087


_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration unk
