# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1496370'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H21 N O'
_chemical_formula_sum            'C24 H21 N O'
_chemical_formula_weight         339.42
_chemical_melting_point          ?
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.2943(19)
_cell_length_b                   18.714(4)
_cell_length_c                   20.557(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.79(3)
_cell_angle_gamma                90.00
_cell_volume                     3557.2(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10313
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4837
_cell_measurement_theta_min      1.9916
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.083
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19024
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.27
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0409
	          2theta: -19.9462
scan:
	Number of images: 240
	           Slice: -110.0000 - 10.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0409
	          2theta: -19.9462
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             8250
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0599
_diffrn_orient_matrix_UB_12      -0.0056
_diffrn_orient_matrix_UB_13      0.0899
_diffrn_orient_matrix_UB_21      -0.0087
_diffrn_orient_matrix_UB_22      -0.0527
_diffrn_orient_matrix_UB_23      0.0025
_diffrn_orient_matrix_UB_31      0.0425
_diffrn_orient_matrix_UB_32      -0.0081
_diffrn_orient_matrix_UB_33      -0.0228
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5618
_reflns_number_total             6173
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    ????
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6173
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0700
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0369P)²+5.1762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1456
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 N2(H2A)
3.b Ternary CH refined with riding coordinates:
 C15(H15), C39(H39)
3.c Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C23(H23A,H23B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C42(H42), C35(H35), C11(H11), C4(H4), C28(H28), C18(H18), C3(H3),
 C9(H9), C34(H34), C8(H8), C43(H43), C27(H27), C10(H10), C25(H25), C32(H32),
 C1(H1A), C33(H33), C2(H2), C44(H44), C26(H26), C19(H19), C20(H20)
3.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C16(H16A,H16B,H16C), C48(H48A,H48B,H48C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O1 O 0.2239(2) 0.31157(10) 0.25008(9) 0.0356(5) Uani 1 d . . . .
O2 O 0.4247(2) 0.16742(10) 0.27949(9) 0.0348(4) Uani 1 d . . . .
N1 N 0.2032(2) 0.20119(11) 0.16288(10) 0.0296(5) Uani 1 d . . . .
H1 H 0.2058 0.1812 0.2017 0.036 Uiso 1 calc . . R .
N2 N 0.2652(2) 0.21862(11) 0.37329(10) 0.0272(5) Uani 1 d . . . .
H2A H 0.2182 0.2201 0.3339 0.033 Uiso 1 d . . R .
C14 C 0.2958(3) 0.31790(14) 0.20367(12) 0.0271(6) Uani 1 d . . . .
C36 C 0.4394(3) 0.31939(14) 0.38697(12) 0.0282(6) Uani 1 d . . . .
C30 C 0.6588(3) 0.31613(16) 0.32608(12) 0.0341(6) Uani 1 d . . . .
C31 C 0.5606(3) 0.35417(15) 0.36655(12) 0.0323(6) Uani 1 d . . . .
C42 C 0.3916(3) 0.07974(14) 0.48518(12) 0.0324(6) Uani 1 d . . . .
H42 H 0.4777 0.0702 0.5127 0.039 Uiso 1 calc . . R .
C38 C 0.4819(3) 0.21492(14) 0.31341(12) 0.0279(6) Uani 1 d . . . .
C5 C 0.3952(3) 0.37883(14) 0.19842(12) 0.0282(6) Uani 1 d . . . .
C15 C 0.1839(3) 0.29723(14) 0.08680(12) 0.0290(6) Uani 1 d . . . .
H15 H 0.2453 0.3188 0.0547 0.035 Uiso 1 calc . . R .
C37 C 0.4173(3) 0.23974(13) 0.37531(11) 0.0251(5) Uani 1 d . . . .
C39 C 0.4904(3) 0.19700(14) 0.43732(12) 0.0273(5) Uani 1 d . . . .
H39 H 0.4903 0.2291 0.4762 0.033 Uiso 1 calc . . R .
C7 C 0.5361(3) 0.30396(14) 0.12747(11) 0.0272(6) Uani 1 d . . . .
C41 C 0.3818(3) 0.13847(13) 0.44465(12) 0.0273(6) Uani 1 d . . . .
C46 C 0.2550(3) 0.15292(13) 0.40505(11) 0.0257(5) Uani 1 d . . . .
C17 C 0.1118(3) 0.23007(15) 0.05880(13) 0.0312(6) Uani 1 d . . . .
C35 C 0.3451(3) 0.35649(15) 0.42272(13) 0.0356(6) Uani 1 d . . . .
H35 H 0.2631 0.3327 0.4365 0.043 Uiso 1 calc . . R .
C11 C 0.4640(3) 0.18272(15) 0.10039(13) 0.0337(6) Uani 1 d . . . .
H11 H 0.3941 0.1456 0.0991 0.040 Uiso 1 calc . . R .
C6 C 0.5081(3) 0.37338(14) 0.15806(12) 0.0279(6) Uani 1 d . . . .
C45 C 0.1356(3) 0.10746(14) 0.40213(13) 0.0308(6) Uani 1 d . . . .
C12 C 0.4325(3) 0.24911(14) 0.12526(12) 0.0260(5) Uani 1 d . . . .
C22 C 0.1226(3) 0.17703(14) 0.10641(13) 0.0316(6) Uani 1 d . . . .
C13 C 0.2829(3) 0.26527(13) 0.14716(12) 0.0257(5) Uani 1 d . . . .
C4 C 0.3762(3) 0.44076(15) 0.23390(14) 0.0379(7) Uani 1 d . . . .
H4 H 0.3017 0.4430 0.2623 0.045 Uiso 1 calc . . R .
C28 C 0.7053(3) 0.21502(18) 0.25692(13) 0.0416(7) Uani 1 d . . . .
H28 H 0.6748 0.1711 0.2368 0.050 Uiso 1 calc . . R .
C18 C 0.0361(3) 0.21779(18) -0.00142(14) 0.0420(7) Uani 1 d . . . .
H18 H 0.0280 0.2538 -0.0342 0.050 Uiso 1 calc . . R .
C3 C 0.4651(3) 0.49892(16) 0.22802(16) 0.0461(8) Uani 1 d . . . .
H3 H 0.4517 0.5414 0.2521 0.055 Uiso 1 calc . . R .
C40 C 0.6449(3) 0.17111(16) 0.43408(14) 0.0363(6) Uani 1 d . . . .
H40A H 0.6485 0.1400 0.3960 0.054 Uiso 1 calc . . GR .
H40B H 0.6768 0.1444 0.4739 0.054 Uiso 1 calc . . GR .
H40C H 0.7086 0.2123 0.4303 0.054 Uiso 1 calc . . GR .
C9 C 0.6993(3) 0.22367(17) 0.07925(13) 0.0393(7) Uani 1 d . . . .
H9 H 0.7903 0.2151 0.0635 0.047 Uiso 1 calc . . R .
C34 C 0.3685(4) 0.42741(16) 0.43864(15) 0.0452(7) Uani 1 d . . . .
H34 H 0.3023 0.4523 0.4628 0.054 Uiso 1 calc . . R .
C29 C 0.6184(3) 0.24971(15) 0.29853(12) 0.0329(6) Uani 1 d . . . .
C47 C 0.0038(3) 0.12293(15) 0.35533(15) 0.0383(7) Uani 1 d . . . .
H47A H 0.0365 0.1392 0.3134 0.046 Uiso 1 calc . . R .
H47B H -0.0496 0.1630 0.3732 0.046 Uiso 1 calc . . R .
C8 C 0.6688(3) 0.28945(16) 0.10397(12) 0.0332(6) Uani 1 d . . . .
H8 H 0.7398 0.3260 0.1051 0.040 Uiso 1 calc . . R .
C43 C 0.2725(3) 0.03454(15) 0.48496(14) 0.0381(7) Uani 1 d . . . .
H43 H 0.2764 -0.0058 0.5131 0.046 Uiso 1 calc . . R .
C27 C 0.8372(3) 0.2452(2) 0.24512(15) 0.0526(9) Uani 1 d . . . .
H27 H 0.8984 0.2213 0.2179 0.063 Uiso 1 calc . . R .
C16 C 0.0708(3) 0.35124(15) 0.10474(14) 0.0353(6) Uani 1 d . . . .
H16A H 0.0048 0.3624 0.0659 0.053 Uiso 1 calc . . GR .
H16B H 0.1193 0.3950 0.1213 0.053 Uiso 1 calc . . GR .
H16C H 0.0159 0.3308 0.1385 0.053 Uiso 1 calc . . GR .
C10 C 0.5972(3) 0.17017(16) 0.07741(14) 0.0397(7) Uani 1 d . . . .
H10 H 0.6180 0.1245 0.0604 0.048 Uiso 1 calc . . R .
C25 C 0.7907(3) 0.3452(2) 0.31217(15) 0.0487(8) Uani 1 d . . . .
H25 H 0.8202 0.3903 0.3301 0.058 Uiso 1 calc . . R .
C21 C 0.0569(3) 0.11045(16) 0.09676(18) 0.0473(8) Uani 1 d . . . .
C32 C 0.5820(4) 0.42595(16) 0.38389(15) 0.0460(8) Uani 1 d . . . .
H32 H 0.6638 0.4504 0.3707 0.055 Uiso 1 calc . . R .
C1 C 0.5965(3) 0.43319(15) 0.15323(14) 0.0375(7) Uani 1 d . . . .
H1A H 0.6735 0.4311 0.1262 0.045 Uiso 1 calc . . R .
C33 C 0.4876(4) 0.46195(17) 0.41953(16) 0.0507(8) Uani 1 d . . . .
H33 H 0.5047 0.5106 0.4309 0.061 Uiso 1 calc . . R .
C2 C 0.5740(4) 0.49509(16) 0.18690(16) 0.0470(8) Uani 1 d . . . .
H2 H 0.6336 0.5355 0.1819 0.056 Uiso 1 calc . . R .
C44 C 0.1481(3) 0.04843(14) 0.44374(14) 0.0364(6) Uani 1 d . . . .
H44 H 0.0686 0.0166 0.4438 0.044 Uiso 1 calc . . R .
C26 C 0.8784(3) 0.3098(2) 0.27305(16) 0.0561(9) Uani 1 d . . . .
H26 H 0.9687 0.3301 0.2652 0.067 Uiso 1 calc . . R .
C48 C -0.0998(4) 0.06130(18) 0.34133(19) 0.0565(9) Uani 1 d . . . .
H48A H -0.1783 0.0759 0.3086 0.085 Uiso 1 calc . . GR .
H48B H -0.1401 0.0473 0.3817 0.085 Uiso 1 calc . . GR .
H48C H -0.0481 0.0207 0.3246 0.085 Uiso 1 calc . . GR .
C19 C -0.0281(3) 0.1511(2) -0.01273(18) 0.0567(10) Uani 1 d . . . .
H19 H -0.0790 0.1411 -0.0541 0.068 Uiso 1 calc . . R .
C20 C -0.0186(3) 0.09945(19) 0.0355(2) 0.0583(10) Uani 1 d . . . .
H20 H -0.0652 0.0548 0.0265 0.070 Uiso 1 calc . . R .
C24 C -0.0506(5) 0.0115(4) 0.1611(3) 0.145(3) Uani 1 d . . . U
H24A H -0.0719 -0.0190 0.1226 0.217 Uiso 1 calc . . GR .
H24B H -0.1356 0.0406 0.1676 0.217 Uiso 1 calc . . GR .
H24C H -0.0259 -0.0185 0.1998 0.217 Uiso 1 calc . . GR .
C23 C 0.0650(4) 0.05585(19) 0.1518(3) 0.0807(14) Uani 1 d . . . U
H23A H 0.1487 0.0246 0.1462 0.097 Uiso 1 calc . . R .
H23B H 0.0888 0.0824 0.1931 0.097 Uiso 1 calc . . R .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C14 1.225(3) . ?
O2 C38 1.218(3) . ?
N1 H1 0.8800 . ?
N1 C22 1.392(3) . ?
N1 C13 1.462(3) . ?
N2 H2A 0.8801 . ?
N2 C37 1.464(3) . ?
N2 C46 1.400(3) . ?
C14 C5 1.479(4) . ?
C14 C13 1.519(4) . ?
C36 C31 1.402(4) . ?
C36 C37 1.521(4) . ?
C36 C35 1.386(4) . ?
C30 C31 1.478(4) . ?
C30 C29 1.401(4) . ?
C30 C25 1.397(4) . ?
C31 C32 1.399(4) . ?
C42 H42 0.9500 . ?
C42 C41 1.377(4) . ?
C42 C43 1.393(4) . ?
C38 C37 1.533(3) . ?
C38 C29 1.486(4) . ?
C5 C6 1.405(4) . ?
C5 C4 1.390(4) . ?
C15 H15 1.0000 . ?
C15 C17 1.511(4) . ?
C15 C13 1.585(3) . ?
C15 C16 1.530(4) . ?
C37 C39 1.597(3) . ?
C39 H39 1.0000 . ?
C39 C41 1.507(4) . ?
C39 C40 1.523(3) . ?
C7 C6 1.478(4) . ?
C7 C12 1.405(3) . ?
C7 C8 1.396(3) . ?
C41 C46 1.390(4) . ?
C46 C45 1.395(4) . ?
C17 C22 1.390(4) . ?
C17 C18 1.380(4) . ?
C35 H35 0.9500 . ?
C35 C34 1.379(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(4) . ?
C11 C10 1.389(4) . ?
C6 C1 1.398(4) . ?
C45 C47 1.507(4) . ?
C45 C44 1.395(4) . ?
C12 C13 1.534(3) . ?
C22 C21 1.393(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.379(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.394(4) . ?
C28 C27 1.393(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.384(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C8 1.372(4) . ?
C9 C10 1.377(4) . ?
C34 H34 0.9500 . ?
C34 C33 1.373(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.511(4) . ?
C8 H8 0.9500 . ?
C43 H43 0.9500 . ?
C43 C44 1.387(4) . ?
C27 H27 0.9500 . ?
C27 C26 1.375(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C10 H10 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.373(5) . ?
C21 C20 1.394(5) . ?
C21 C23 1.521(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.375(5) . ?
C1 H1A 0.9500 . ?
C1 C2 1.376(4) . ?
C33 H33 0.9500 . ?
C2 H2 0.9500 . ?
C44 H44 0.9500 . ?
C26 H26 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.381(5) . ?
C20 H20 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 C23 1.386(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 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
C22 N1 H1 125.5 . . ?
C22 N1 C13 108.9(2) . . ?
C13 N1 H1 125.5 . . ?
C37 N2 H2A 113.9 . . ?
C46 N2 H2A 113.9 . . ?
C46 N2 C37 109.54(19) . . ?
O1 C14 C5 121.7(2) . . ?
O1 C14 C13 121.7(2) . . ?
C5 C14 C13 116.5(2) . . ?
C31 C36 C37 120.5(2) . . ?
C35 C36 C31 119.8(3) . . ?
C35 C36 C37 119.5(2) . . ?
C29 C30 C31 120.0(2) . . ?
C25 C30 C31 122.1(3) . . ?
C25 C30 C29 117.9(3) . . ?
C36 C31 C30 120.4(2) . . ?
C32 C31 C36 117.9(3) . . ?
C32 C31 C30 121.7(3) . . ?
C41 C42 H42 120.7 . . ?
C41 C42 C43 118.6(3) . . ?
C43 C42 H42 120.7 . . ?
O2 C38 C37 120.8(2) . . ?
O2 C38 C29 122.3(2) . . ?
C29 C38 C37 116.9(2) . . ?
C6 C5 C14 119.8(2) . . ?
C4 C5 C14 119.4(2) . . ?
C4 C5 C6 120.8(2) . . ?
C17 C15 H15 110.2 . . ?
C17 C15 C13 100.6(2) . . ?
C17 C15 C16 110.6(2) . . ?
C13 C15 H15 110.2 . . ?
C16 C15 H15 110.2 . . ?
C16 C15 C13 114.8(2) . . ?
N2 C37 C36 112.6(2) . . ?
N2 C37 C38 110.6(2) . . ?
N2 C37 C39 102.67(18) . . ?
C36 C37 C38 111.7(2) . . ?
C36 C37 C39 109.0(2) . . ?
C38 C37 C39 109.88(19) . . ?
C37 C39 H39 107.6 . . ?
C41 C39 C37 102.03(19) . . ?
C41 C39 H39 107.6 . . ?
C41 C39 C40 114.6(2) . . ?
C40 C39 C37 116.8(2) . . ?
C40 C39 H39 107.6 . . ?
C12 C7 C6 120.4(2) . . ?
C8 C7 C6 121.2(2) . . ?
C8 C7 C12 118.3(2) . . ?
C42 C41 C39 129.6(2) . . ?
C42 C41 C46 120.6(2) . . ?
C46 C41 C39 109.7(2) . . ?
C41 C46 N2 110.5(2) . . ?
C41 C46 C45 122.1(2) . . ?
C45 C46 N2 127.3(2) . . ?
C22 C17 C15 109.1(2) . . ?
C18 C17 C15 130.3(3) . . ?
C18 C17 C22 120.4(3) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 C36 121.0(3) . . ?
C34 C35 H35 119.5 . . ?
C12 C11 H11 119.8 . . ?
C12 C11 C10 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C5 C6 C7 119.3(2) . . ?
C1 C6 C5 117.6(2) . . ?
C1 C6 C7 122.9(2) . . ?
C46 C45 C47 120.1(2) . . ?
C46 C45 C44 116.1(2) . . ?
C44 C45 C47 123.8(2) . . ?
C7 C12 C13 119.0(2) . . ?
C11 C12 C7 119.8(2) . . ?
C11 C12 C13 121.1(2) . . ?
N1 C22 C21 126.9(3) . . ?
C17 C22 N1 110.5(2) . . ?
C17 C22 C21 122.6(3) . . ?
N1 C13 C14 111.45(19) . . ?
N1 C13 C15 102.45(19) . . ?
N1 C13 C12 113.4(2) . . ?
C14 C13 C15 110.4(2) . . ?
C14 C13 C12 110.4(2) . . ?
C12 C13 C15 108.42(19) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C27 C28 C29 119.5(3) . . ?
C17 C18 H18 121.0 . . ?
C17 C18 C19 118.0(3) . . ?
C19 C18 H18 121.0 . . ?
C4 C3 H3 120.2 . . ?
C4 C3 C2 119.6(3) . . ?
C2 C3 H3 120.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(2) . . ?
C10 C9 H9 120.2 . . ?
C35 C34 H34 120.1 . . ?
C33 C34 C35 119.8(3) . . ?
C33 C34 H34 120.1 . . ?
C30 C29 C38 120.3(2) . . ?
C28 C29 C30 120.9(3) . . ?
C28 C29 C38 118.8(3) . . ?
C45 C47 H47A 108.3 . . ?
C45 C47 H47B 108.3 . . ?
C45 C47 C48 115.8(3) . . ?
H47A C47 H47B 107.4 . . ?
C48 C47 H47A 108.3 . . ?
C48 C47 H47B 108.3 . . ?
C7 C8 H8 119.2 . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.2 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 C42 120.1(2) . . ?
C44 C43 H43 120.0 . . ?
C28 C27 H27 120.1 . . ?
C26 C27 C28 119.8(3) . . ?
C26 C27 H27 120.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C10 H10 119.9 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C30 C25 H25 119.4 . . ?
C26 C25 C30 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C22 C21 C20 115.7(3) . . ?
C22 C21 C23 120.5(3) . . ?
C20 C21 C23 123.8(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.6(3) . . ?
C33 C32 H32 119.2 . . ?
C6 C1 H1A 119.4 . . ?
C2 C1 C6 121.2(3) . . ?
C2 C1 H1A 119.4 . . ?
C34 C33 H33 120.1 . . ?
C32 C33 C34 119.9(3) . . ?
C32 C33 H33 120.1 . . ?
C3 C2 H2 119.7 . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
C45 C44 H44 118.8 . . ?
C43 C44 C45 122.4(3) . . ?
C43 C44 H44 118.8 . . ?
C27 C26 H26 119.6 . . ?
C25 C26 C27 120.8(3) . . ?
C25 C26 H26 119.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.9(3) . . ?
C20 C19 H19 119.6 . . ?
C21 C20 H20 118.8 . . ?
C19 C20 C21 122.3(3) . . ?
C19 C20 H20 118.8 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
C21 C23 H23A 106.9 . . ?
C21 C23 H23B 106.9 . . ?
C24 C23 C21 121.6(4) . . ?
C24 C23 H23A 106.9 . . ?
C24 C23 H23B 106.9 . . ?
H23A C23 H23B 106.7 . . ?

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
O1 C14 C5 C6 159.3(2) . . . . ?
O1 C14 C5 C4 -20.4(4) . . . . ?
O1 C14 C13 N1 -12.8(3) . . . . ?
O1 C14 C13 C15 100.4(3) . . . . ?
O1 C14 C13 C12 -139.7(2) . . . . ?
O2 C38 C37 N2 -19.6(3) . . . . ?
O2 C38 C37 C36 -145.9(2) . . . . ?
O2 C38 C37 C39 93.1(3) . . . . ?
O2 C38 C29 C30 161.6(2) . . . . ?
O2 C38 C29 C28 -18.5(4) . . . . ?
N1 C22 C21 C20 179.7(3) . . . . ?
N1 C22 C21 C23 1.9(4) . . . . ?
N2 C37 C39 C41 20.6(2) . . . . ?
N2 C37 C39 C40 146.4(2) . . . . ?
N2 C46 C45 C47 7.1(4) . . . . ?
N2 C46 C45 C44 -173.6(2) . . . . ?
C14 C5 C6 C7 -7.0(3) . . . . ?
C14 C5 C6 C1 178.1(2) . . . . ?
C14 C5 C4 C3 -178.0(2) . . . . ?
C36 C31 C32 C33 -0.3(4) . . . . ?
C36 C37 C39 C41 140.2(2) . . . . ?
C36 C37 C39 C40 -94.0(3) . . . . ?
C36 C35 C34 C33 -0.7(5) . . . . ?
C30 C31 C32 C33 177.6(3) . . . . ?
C30 C25 C26 C27 1.6(5) . . . . ?
C31 C36 C37 N2 -155.7(2) . . . . ?
C31 C36 C37 C38 -30.4(3) . . . . ?
C31 C36 C37 C39 91.1(3) . . . . ?
C31 C36 C35 C34 0.0(4) . . . . ?
C31 C30 C29 C38 -4.1(4) . . . . ?
C31 C30 C29 C28 176.0(2) . . . . ?
C31 C30 C25 C26 -178.3(3) . . . . ?
C31 C32 C33 C34 -0.3(5) . . . . ?
C42 C41 C46 N2 174.1(2) . . . . ?
C42 C41 C46 C45 -3.1(4) . . . . ?
C42 C43 C44 C45 -0.9(4) . . . . ?
C38 C37 C39 C41 -97.1(2) . . . . ?
C38 C37 C39 C40 28.7(3) . . . . ?
C5 C14 C13 N1 169.7(2) . . . . ?
C5 C14 C13 C15 -77.2(3) . . . . ?
C5 C14 C13 C12 42.7(3) . . . . ?
C5 C6 C1 C2 0.1(4) . . . . ?
C5 C4 C3 C2 -0.4(4) . . . . ?
C15 C17 C22 N1 -3.5(3) . . . . ?
C15 C17 C22 C21 175.2(2) . . . . ?
C15 C17 C18 C19 -175.7(3) . . . . ?
C37 N2 C46 C41 17.7(3) . . . . ?
C37 N2 C46 C45 -165.3(2) . . . . ?
C37 C36 C31 C30 7.8(4) . . . . ?
C37 C36 C31 C32 -174.3(2) . . . . ?
C37 C36 C35 C34 174.8(3) . . . . ?
C37 C38 C29 C30 -20.4(3) . . . . ?
C37 C38 C29 C28 159.5(2) . . . . ?
C37 C39 C41 C42 172.0(2) . . . . ?
C37 C39 C41 C46 -11.5(3) . . . . ?
C39 C41 C46 N2 -2.8(3) . . . . ?
C39 C41 C46 C45 -180.0(2) . . . . ?
C7 C6 C1 C2 -174.5(3) . . . . ?
C7 C12 C13 N1 -161.2(2) . . . . ?
C7 C12 C13 C14 -35.4(3) . . . . ?
C7 C12 C13 C15 85.7(3) . . . . ?
C41 C42 C43 C44 1.0(4) . . . . ?
C41 C46 C45 C47 -176.2(2) . . . . ?
C41 C46 C45 C44 3.1(4) . . . . ?
C46 N2 C37 C36 -140.7(2) . . . . ?
C46 N2 C37 C38 93.5(2) . . . . ?
C46 N2 C37 C39 -23.7(2) . . . . ?
C46 C45 C47 C48 162.8(3) . . . . ?
C46 C45 C44 C43 -1.1(4) . . . . ?
C17 C15 C13 N1 -27.3(2) . . . . ?
C17 C15 C13 C14 -146.1(2) . . . . ?
C17 C15 C13 C12 92.9(2) . . . . ?
C17 C22 C21 C20 1.3(4) . . . . ?
C17 C22 C21 C23 -176.5(3) . . . . ?
C17 C18 C19 C20 1.4(4) . . . . ?
C35 C36 C31 C30 -177.5(2) . . . . ?
C35 C36 C31 C32 0.5(4) . . . . ?
C35 C36 C37 N2 29.6(3) . . . . ?
C35 C36 C37 C38 154.8(2) . . . . ?
C35 C36 C37 C39 -83.6(3) . . . . ?
C35 C34 C33 C32 0.8(5) . . . . ?
C11 C12 C13 N1 22.1(3) . . . . ?
C11 C12 C13 C14 148.0(2) . . . . ?
C11 C12 C13 C15 -91.0(3) . . . . ?
C6 C5 C4 C3 2.4(4) . . . . ?
C6 C7 C12 C11 -175.7(2) . . . . ?
C6 C7 C12 C13 7.6(3) . . . . ?
C6 C7 C8 C9 175.8(2) . . . . ?
C6 C1 C2 C3 1.8(4) . . . . ?
C12 C7 C6 C5 15.3(3) . . . . ?
C12 C7 C6 C1 -170.2(2) . . . . ?
C12 C7 C8 C9 -0.1(4) . . . . ?
C12 C11 C10 C9 0.1(4) . . . . ?
C22 N1 C13 C14 145.4(2) . . . . ?
C22 N1 C13 C15 27.3(2) . . . . ?
C22 N1 C13 C12 -89.3(2) . . . . ?
C22 C17 C18 C19 -0.1(4) . . . . ?
C22 C21 C20 C19 -0.1(4) . . . . ?
C22 C21 C23 C24 142.8(5) . . . . ?
C13 N1 C22 C17 -16.0(3) . . . . ?
C13 N1 C22 C21 165.4(3) . . . . ?
C13 C14 C5 C6 -23.2(3) . . . . ?
C13 C14 C5 C4 157.2(2) . . . . ?
C13 C15 C17 C22 19.4(2) . . . . ?
C13 C15 C17 C18 -164.7(3) . . . . ?
C4 C5 C6 C7 172.6(2) . . . . ?
C4 C5 C6 C1 -2.2(4) . . . . ?
C4 C3 C2 C1 -1.7(5) . . . . ?
C28 C27 C26 C25 -0.5(5) . . . . ?
C18 C17 C22 N1 -179.9(2) . . . . ?
C18 C17 C22 C21 -1.2(4) . . . . ?
C18 C19 C20 C21 -1.3(5) . . . . ?
C40 C39 C41 C42 44.7(4) . . . . ?
C40 C39 C41 C46 -138.7(2) . . . . ?
C29 C30 C31 C36 11.0(4) . . . . ?
C29 C30 C31 C32 -166.9(3) . . . . ?
C29 C30 C25 C26 -0.3(4) . . . . ?
C29 C38 C37 N2 162.4(2) . . . . ?
C29 C38 C37 C36 36.1(3) . . . . ?
C29 C38 C37 C39 -84.9(3) . . . . ?
C29 C28 C27 C26 -1.8(4) . . . . ?
C47 C45 C44 C43 178.1(3) . . . . ?
C8 C7 C6 C5 -160.5(2) . . . . ?
C8 C7 C6 C1 14.0(4) . . . . ?
C8 C7 C12 C11 0.2(4) . . . . ?
C8 C7 C12 C13 -176.5(2) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C43 C42 C41 C39 177.1(2) . . . . ?
C43 C42 C41 C46 0.9(4) . . . . ?
C27 C28 C29 C30 3.1(4) . . . . ?
C27 C28 C29 C38 -176.8(2) . . . . ?
C16 C15 C17 C22 -102.3(2) . . . . ?
C16 C15 C17 C18 73.6(3) . . . . ?
C16 C15 C13 N1 91.4(2) . . . . ?
C16 C15 C13 C14 -27.4(3) . . . . ?
C16 C15 C13 C12 -148.4(2) . . . . ?
C10 C11 C12 C7 -0.3(4) . . . . ?
C10 C11 C12 C13 176.4(2) . . . . ?
C10 C9 C8 C7 -0.1(4) . . . . ?
C25 C30 C31 C36 -171.1(3) . . . . ?
C25 C30 C31 C32 11.0(4) . . . . ?
C25 C30 C29 C38 177.9(2) . . . . ?
C25 C30 C29 C28 -2.0(4) . . . . ?
C44 C45 C47 C48 -16.4(4) . . . . ?
C20 C21 C23 C24 -34.8(7) . . . . ?
C23 C21 C20 C19 177.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1496371'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H19 N'
_chemical_formula_sum            'C24 H19 N'
_chemical_formula_weight         321.40
_chemical_melting_point          ?
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 'x, -y-1/2, z-1/2'
8 '-x-1/2, y-1/2, z'

_cell_length_a                   11.335(2)
_cell_length_b                   7.4991(15)
_cell_length_c                   37.869(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3218.9(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8542
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4827
_cell_measurement_theta_min      1.0754
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6506
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.031
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11343
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.80
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 15.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 50.2452
	          2theta: -20.0323
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             4206
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0146
_diffrn_orient_matrix_UB_12      0.1155
_diffrn_orient_matrix_UB_13      -0.0650
_diffrn_orient_matrix_UB_21      0.0737
_diffrn_orient_matrix_UB_22      0.0164
_diffrn_orient_matrix_UB_23      0.0456
_diffrn_orient_matrix_UB_31      0.0142
_diffrn_orient_matrix_UB_32      -0.0123
_diffrn_orient_matrix_UB_33      -0.0186
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3277
_reflns_number_total             3672
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    ????
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3672
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0693
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0408P)²+2.2429P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1441
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23B,H23A)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C18(H18), C20(H20), C10(H10), C2(H2), C5(H5), C11(H11), C9(H9),
 C19(H19), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16C,H16B), C24(H24B,H24A,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
N1 N 0.36770(14) 0.2064(2) 0.58936(4) 0.0227(4) Uani 1 d . . .
C17 C 0.15722(17) 0.2174(3) 0.60099(5) 0.0227(4) Uani 1 d . . .
C22 C 0.25425(17) 0.1799(3) 0.57856(5) 0.0229(4) Uani 1 d . . .
C14 C 0.38634(16) 0.2523(3) 0.62266(5) 0.0213(4) Uani 1 d . . .
C8 C 0.47370(18) 0.3777(3) 0.72993(5) 0.0296(5) Uani 1 d . . .
H8 H 0.5490 0.4249 0.7358 0.036 Uiso 1 calc . . R
C6 C 0.53397(16) 0.3667(3) 0.66614(5) 0.0233(4) Uani 1 d . . .
C13 C 0.29521(16) 0.2681(3) 0.64858(5) 0.0215(4) Uani 1 d . . .
C15 C 0.17843(16) 0.2673(3) 0.63655(5) 0.0220(4) Uani 1 d . . .
C1 C 0.50834(16) 0.3037(3) 0.63202(5) 0.0222(4) Uani 1 d . . .
C18 C 0.04093(17) 0.1978(3) 0.58703(5) 0.0275(5) Uani 1 d . . .
H18 H -0.0256 0.2244 0.6014 0.033 Uiso 1 calc . . R
C21 C 0.23623(17) 0.1218(3) 0.54290(5) 0.0243(4) Uani 1 d . . .
C20 C 0.12258(18) 0.1035(3) 0.53127(5) 0.0288(5) Uani 1 d . . .
H20 H 0.1088 0.0645 0.5078 0.035 Uiso 1 calc . . R
C7 C 0.44511(17) 0.3484(3) 0.69425(5) 0.0240(4) Uani 1 d . . .
C10 C 0.28601(18) 0.2628(3) 0.74840(5) 0.0294(5) Uani 1 d . . .
H10 H 0.2336 0.2280 0.7667 0.035 Uiso 1 calc . . R
C2 C 0.59637(17) 0.3056(3) 0.60608(5) 0.0273(5) Uani 1 d . . .
H2 H 0.5798 0.2595 0.5832 0.033 Uiso 1 calc . . R
C12 C 0.33009(16) 0.2886(3) 0.68577(5) 0.0222(4) Uani 1 d . . .
C16 C 0.07566(17) 0.3317(3) 0.65851(5) 0.0258(4) Uani 1 d . . .
H16A H 0.0229 0.4037 0.6438 0.039 Uiso 1 calc . . GR
H16C H 0.1050 0.4042 0.6782 0.039 Uiso 1 calc . . GR
H16B H 0.0324 0.2288 0.6678 0.039 Uiso 1 calc . . GR
C24 C 0.3164(2) 0.0170(3) 0.48306(5) 0.0337(5) Uani 1 d . . .
H24B H 0.3906 -0.0032 0.4704 0.051 Uiso 1 calc . . GR
H24A H 0.2693 0.1060 0.4704 0.051 Uiso 1 calc . . GR
H24C H 0.2722 -0.0951 0.4845 0.051 Uiso 1 calc . . GR
C23 C 0.34290(18) 0.0843(3) 0.52026(5) 0.0287(5) Uani 1 d . . .
H23B H 0.3924 -0.0054 0.5324 0.034 Uiso 1 calc . . R
H23A H 0.3899 0.1952 0.5183 0.034 Uiso 1 calc . . R
C5 C 0.64649(17) 0.4387(3) 0.67259(6) 0.0276(5) Uani 1 d . . .
H5 H 0.6644 0.4849 0.6953 0.033 Uiso 1 calc . . R
C11 C 0.25483(18) 0.2379(3) 0.71358(5) 0.0261(4) Uani 1 d . . .
H11 H 0.1807 0.1853 0.7082 0.031 Uiso 1 calc . . R
C9 C 0.39461(19) 0.3391(3) 0.75666(5) 0.0326(5) Uani 1 d . . .
H9 H 0.4142 0.3645 0.7805 0.039 Uiso 1 calc . . R
C19 C 0.02525(18) 0.1411(3) 0.55327(6) 0.0297(5) Uani 1 d . . .
H19 H -0.0525 0.1265 0.5443 0.036 Uiso 1 calc . . R
C4 C 0.73114(17) 0.4435(3) 0.64656(6) 0.0312(5) Uani 1 d . . .
H4 H 0.8062 0.4946 0.6513 0.037 Uiso 1 calc . . R
C3 C 0.70706(18) 0.3739(3) 0.61330(6) 0.0315(5) Uani 1 d . . .
H3 H 0.7665 0.3732 0.5956 0.038 Uiso 1 calc . . R


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C22 1.364(2) . ?
N1 C14 1.324(2) . ?
C17 C22 1.418(3) . ?
C17 C15 1.418(3) . ?
C17 C18 1.428(3) . ?
C22 C21 1.434(3) . ?
C14 C13 1.430(3) . ?
C14 C1 1.479(3) . ?
C8 C7 1.407(3) . ?
C8 C9 1.383(3) . ?
C6 C1 1.406(3) . ?
C6 C7 1.472(3) . ?
C6 C5 1.406(3) . ?
C13 C15 1.400(3) . ?
C13 C12 1.471(3) . ?
C15 C16 1.510(3) . ?
C1 C2 1.401(3) . ?
C18 C19 1.359(3) . ?
C21 C20 1.368(3) . ?
C21 C23 1.508(3) . ?
C20 C19 1.411(3) . ?
C7 C12 1.416(3) . ?
C10 C11 1.378(3) . ?
C10 C9 1.393(3) . ?
C2 C3 1.382(3) . ?
C12 C11 1.408(3) . ?
C24 C23 1.526(3) . ?
C5 C4 1.376(3) . ?
C4 C3 1.390(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
C14 N1 C22 118.27(16) . . ?
C22 C17 C15 119.32(17) . . ?
C22 C17 C18 118.29(18) . . ?
C15 C17 C18 122.36(18) . . ?
N1 C22 C17 121.53(17) . . ?
N1 C22 C21 117.45(17) . . ?
C17 C22 C21 120.94(18) . . ?
N1 C14 C13 124.06(17) . . ?
N1 C14 C1 116.44(17) . . ?
C13 C14 C1 119.30(17) . . ?
C9 C8 C7 121.4(2) . . ?
C1 C6 C7 119.48(17) . . ?
C1 C6 C5 118.42(18) . . ?
C5 C6 C7 122.05(18) . . ?
C14 C13 C12 118.15(17) . . ?
C15 C13 C14 117.36(17) . . ?
C15 C13 C12 124.47(17) . . ?
C17 C15 C16 118.44(17) . . ?
C13 C15 C17 118.05(17) . . ?
C13 C15 C16 123.30(17) . . ?
C6 C1 C14 120.08(17) . . ?
C2 C1 C14 120.05(18) . . ?
C2 C1 C6 119.61(18) . . ?
C19 C18 C17 120.08(19) . . ?
C22 C21 C23 118.54(17) . . ?
C20 C21 C22 117.88(19) . . ?
C20 C21 C23 123.58(19) . . ?
C21 C20 C19 121.75(19) . . ?
C8 C7 C6 121.51(18) . . ?
C8 C7 C12 118.65(18) . . ?
C12 C7 C6 119.70(17) . . ?
C11 C10 C9 119.8(2) . . ?
C3 C2 C1 120.76(19) . . ?
C7 C12 C13 119.87(17) . . ?
C11 C12 C13 121.69(17) . . ?
C11 C12 C7 118.28(18) . . ?
C21 C23 C24 115.36(17) . . ?
C4 C5 C6 121.20(19) . . ?
C10 C11 C12 121.61(19) . . ?
C8 C9 C10 119.6(2) . . ?
C18 C19 C20 121.05(18) . . ?
C5 C4 C3 120.14(19) . . ?
C2 C3 C4 119.77(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Pd1
_database_code_depnum_ccdc_archive 'CCDC 1496372'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H34 Cl7 N3 Pd'
_chemical_formula_weight         935.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9990 1.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.641(2)
_cell_length_b                   10.978(2)
_cell_length_c                   17.744(3)
_cell_angle_alpha                100.04(3)
_cell_angle_beta                 106.43(3)
_cell_angle_gamma                93.41(3)
_cell_volume                     1944.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6719
_cell_measurement_theta_min      1.8966
_cell_measurement_theta_max      27.4696

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6158
_exptl_absorpt_correction_T_max  0.8900

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24363
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         27.47
_reflns_number_total             8870
_reflns_number_gt                8566
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1530P)²+9.8860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8870
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2352
_refine_ls_wR_factor_gt          0.2212
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001

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 0.53800(3) 0.50295(3) 0.66307(2) 0.02381(15) Uani 1 1 d . . .
Cl1 Cl 0.64385(15) 0.69623(13) 0.73395(9) 0.0381(3) Uani 1 1 d . . .
N1 N 0.4439(4) 0.3411(4) 0.5891(2) 0.0228(8) Uani 1 1 d . . .
N3 N 0.1552(4) -0.0192(4) 0.3668(3) 0.0267(8) Uani 1 1 d . . .
N2 N 0.4286(4) 0.4792(4) 0.7438(2) 0.0259(8) Uani 1 1 d . . .
C12 C 0.4503(5) 0.1902(5) 0.4723(3) 0.0238(9) Uani 1 1 d . . .
C1 C 0.6510(5) 0.4880(5) 0.5912(3) 0.0253(9) Uani 1 1 d . . .
C11 C 0.5361(5) 0.1389(5) 0.4271(3) 0.0253(9) Uani 1 1 d . . .
C28 C 0.6308(6) 0.5678(6) 0.9578(3) 0.0384(13) Uani 1 1 d . . .
H28 H 0.6989 0.5385 0.9954 0.046 Uiso 1 1 calc R . .
C38 C 0.0951(5) -0.1984(5) 0.2579(3) 0.0299(10) Uani 1 1 d . . .
C6 C 0.6550(5) 0.2099(5) 0.4312(3) 0.0282(10) Uani 1 1 d . . .
C13 C 0.5030(5) 0.2978(5) 0.5334(3) 0.0235(9) Uani 1 1 d . . .
C33 C 0.0833(5) -0.0746(5) 0.2861(3) 0.0261(10) Uani 1 1 d . . .
C16 C 0.2514(5) 0.1941(5) 0.5152(3) 0.0255(9) Uani 1 1 d . . .
C5 C 0.6908(5) 0.3338(5) 0.4822(3) 0.0272(10) Uani 1 1 d . . .
C17 C 0.1173(5) 0.1521(5) 0.5042(3) 0.0297(10) Uani 1 1 d . . .
H17 H 0.0695 0.0925 0.4577 0.036 Uiso 1 1 calc R . .
C20 C 0.2602(5) 0.3225(5) 0.6464(3) 0.0279(10) Uani 1 1 d . . .
C14 C 0.6194(5) 0.3733(5) 0.5358(3) 0.0252(9) Uani 1 1 d . . .
C19 C 0.1294(5) 0.2777(5) 0.6314(3) 0.0326(11) Uani 1 1 d . . .
H19 H 0.0872 0.3028 0.6712 0.039 Uiso 1 1 calc R . .
C15 C 0.3174(5) 0.1471(4) 0.4584(3) 0.0238(9) Uani 1 1 d . . .
C3 C 0.8304(6) 0.5304(6) 0.5367(4) 0.0360(12) Uani 1 1 d . . .
H3 H 0.9024 0.5854 0.5363 0.043 Uiso 1 1 calc R . .
C2 C 0.7601(5) 0.5669(5) 0.5912(4) 0.0320(11) Uani 1 1 d . . .
H2 H 0.7860 0.6445 0.6280 0.038 Uiso 1 1 calc R . .
C10 C 0.5081(5) 0.0157(5) 0.3833(3) 0.0300(10) Uani 1 1 d . . .
H10 H 0.4315 -0.0339 0.3828 0.036 Uiso 1 1 calc R . .
C24 C 0.4833(5) 0.5458(5) 0.8252(3) 0.0269(10) Uani 1 1 d . . .
C18 C 0.0566(5) 0.1964(5) 0.5599(3) 0.0319(11) Uani 1 1 d . . .
H18 H -0.0348 0.1725 0.5503 0.038 Uiso 1 1 calc R . .
C34 C -0.0028(5) -0.0067(6) 0.2387(4) 0.0329(11) Uani 1 1 d . . .
C29 C 0.5839(6) 0.5017(5) 0.8784(3) 0.0321(11) Uani 1 1 d . . .
C22 C 0.3280(5) 0.3967(5) 0.7281(3) 0.0280(10) Uani 1 1 d . . .
C7 C 0.7372(5) 0.1558(6) 0.3889(3) 0.0333(11) Uani 1 1 d . . .
H7 H 0.8166 0.2028 0.3913 0.040 Uiso 1 1 calc R . .
C37 C 0.0215(6) -0.2549(6) 0.1793(4) 0.0379(13) Uani 1 1 d . . .
H37 H 0.0303 -0.3389 0.1588 0.046 Uiso 1 1 calc R . .
C21 C 0.3213(5) 0.2865(5) 0.5842(3) 0.0245(9) Uani 1 1 d . . .
C4 C 0.7984(5) 0.4174(6) 0.4836(4) 0.0331(11) Uani 1 1 d . . .
H4 H 0.8488 0.3955 0.4479 0.040 Uiso 1 1 calc R . .
C30 C 0.6380(7) 0.3839(6) 0.8525(4) 0.0470(16) Uani 1 1 d . . .
H30A H 0.6856 0.3968 0.8141 0.070 Uiso 1 1 calc R . .
H30B H 0.5653 0.3170 0.8270 0.070 Uiso 1 1 calc R . .
H30C H 0.6984 0.3607 0.8993 0.070 Uiso 1 1 calc R . .
C25 C 0.4301(6) 0.6565(5) 0.8482(3) 0.0326(11) Uani 1 1 d . . .
C8 C 0.7067(6) 0.0373(6) 0.3443(4) 0.0374(12) Uani 1 1 d . . .
H8 H 0.7639 0.0037 0.3156 0.045 Uiso 1 1 calc R . .
C27 C 0.5792(7) 0.6747(6) 0.9819(3) 0.0433(14) Uani 1 1 d . . .
H27 H 0.6122 0.7186 1.0359 0.052 Uiso 1 1 calc R . .
C26 C 0.4795(7) 0.7191(6) 0.9282(4) 0.0386(13) Uani 1 1 d . . .
H26 H 0.4445 0.7926 0.9459 0.046 Uiso 1 1 calc R . .
C9 C 0.5907(6) -0.0346(6) 0.3409(4) 0.0359(12) Uani 1 1 d . . .
H9 H 0.5690 -0.1169 0.3099 0.043 Uiso 1 1 calc R . .
C40 C -0.0146(7) 0.1262(6) 0.2672(4) 0.0450(15) Uani 1 1 d . . .
H40A H -0.0170 0.1389 0.3228 0.068 Uiso 1 1 calc R . .
H40B H -0.0959 0.1494 0.2333 0.068 Uiso 1 1 calc R . .
H40C H 0.0614 0.1782 0.2644 0.068 Uiso 1 1 calc R . .
C36 C -0.0631(7) -0.1901(7) 0.1316(4) 0.0447(15) Uani 1 1 d . . .
H36 H -0.1118 -0.2288 0.0782 0.054 Uiso 1 1 calc R . .
C31 C 0.3258(7) 0.7044(7) 0.7880(4) 0.0450(15) Uani 1 1 d . . .
H31A H 0.3617 0.7260 0.7463 0.067 Uiso 1 1 calc R . .
H31B H 0.2970 0.7787 0.8148 0.067 Uiso 1 1 calc R . .
H31C H 0.2504 0.6400 0.7636 0.067 Uiso 1 1 calc R . .
C35 C -0.0773(6) -0.0679(7) 0.1618(4) 0.0426(14) Uani 1 1 d . . .
H35 H -0.1392 -0.0251 0.1294 0.051 Uiso 1 1 calc R . .
C23 C 0.2728(7) 0.3684(7) 0.7940(4) 0.0421(14) Uani 1 1 d . . .
H23A H 0.3417 0.3914 0.8457 0.063 Uiso 1 1 calc R . .
H23B H 0.2428 0.2792 0.7833 0.063 Uiso 1 1 calc R . .
H23C H 0.1984 0.4162 0.7954 0.063 Uiso 1 1 calc R . .
C39 C 0.1902(7) -0.2681(6) 0.3111(4) 0.0398(13) Uani 1 1 d . . .
H39A H 0.2807 -0.2412 0.3130 0.060 Uiso 1 1 calc R . .
H39B H 0.1697 -0.3577 0.2892 0.060 Uiso 1 1 calc R . .
H39C H 0.1815 -0.2503 0.3653 0.060 Uiso 1 1 calc R . .
C32 C 0.2441(5) 0.0696(5) 0.3785(3) 0.0253(9) Uani 1 1 d . . .
H32 H 0.2656 0.0882 0.3330 0.030 Uiso 1 1 calc R . .
Cl7 Cl 0.0308(12) 0.1868(6) 0.0789(4) 0.260(6) Uani 1 1 d . . .
Cl5 Cl 0.0170(6) 0.4087(4) 0.1955(3) 0.1296(15) Uani 1 1 d . . .
Cl6 Cl 0.0197(6) 0.4331(5) 0.0355(3) 0.1475(17) Uani 1 1 d . . .
C42 C 0.0690(13) 0.3406(12) 0.1145(7) 0.084(3) Uani 1 1 d . . .
H42 H 0.1676 0.3546 0.1339 0.100 Uiso 1 1 calc R . .
Cl2 Cl 0.28437(18) 0.94353(18) 0.17305(11) 0.0515(4) Uani 1 1 d . . .
Cl3 Cl 0.5240(2) 0.9570(2) 0.12604(14) 0.0625(5) Uani 1 1 d . . .
C41 C 0.3749(8) 1.0237(7) 0.1253(4) 0.0494(16) Uani 1 1 d . . .
H41 H 0.3965 1.1129 0.1535 0.059 Uiso 1 1 calc R . .
Cl4 Cl 0.2841(3) 1.0152(4) 0.02495(17) 0.1111(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.979(5) . ?
Pd1 N1 2.028(4) . ?
Pd1 N2 2.123(4) . ?
Pd1 Cl1 2.3100(17) . ?
N1 C13 1.349(6) . ?
N1 C21 1.376(6) . ?
N3 C32 1.264(7) . ?
N3 C33 1.424(6) . ?
N2 C22 1.294(7) . ?
N2 C24 1.438(6) . ?
C12 C15 1.402(7) . ?
C12 C13 1.420(7) . ?
C12 C11 1.455(7) . ?
C1 C2 1.407(7) . ?
C1 C14 1.413(7) . ?
C11 C10 1.405(8) . ?
C11 C6 1.423(7) . ?
C28 C27 1.377(9) . ?
C28 C29 1.401(8) . ?
C28 H28 0.9500 . ?
C38 C33 1.390(8) . ?
C38 C37 1.402(8) . ?
C38 C39 1.518(8) . ?
C6 C7 1.399(7) . ?
C6 C5 1.460(8) . ?
C13 C14 1.436(7) . ?
C33 C34 1.403(7) . ?
C16 C17 1.422(7) . ?
C16 C21 1.429(7) . ?
C16 C15 1.428(7) . ?
C5 C14 1.404(7) . ?
C5 C4 1.415(7) . ?
C17 C18 1.363(7) . ?
C17 H17 0.9500 . ?
C20 C19 1.383(7) . ?
C20 C21 1.442(7) . ?
C20 C22 1.488(7) . ?
C19 C18 1.405(8) . ?
C19 H19 0.9500 . ?
C15 C32 1.489(7) . ?
C3 C4 1.380(9) . ?
C3 C2 1.402(8) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
C10 C9 1.390(8) . ?
C10 H10 0.9500 . ?
C24 C29 1.386(8) . ?
C24 C25 1.415(7) . ?
C18 H18 0.9500 . ?
C34 C35 1.395(8) . ?
C34 C40 1.484(9) . ?
C29 C30 1.499(8) . ?
C22 C23 1.516(7) . ?
C7 C8 1.366(9) . ?
C7 H7 0.9500 . ?
C37 C36 1.374(10) . ?
C37 H37 0.9500 . ?
C4 H4 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C25 C26 1.400(8) . ?
C25 C31 1.498(8) . ?
C8 C9 1.406(9) . ?
C8 H8 0.9500 . ?
C27 C26 1.386(9) . ?
C27 H27 0.9500 . ?
C26 H26 0.9500 . ?
C9 H9 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C36 C35 1.389(10) . ?
C36 H36 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C35 H35 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C32 H32 0.9500 . ?
Cl7 C42 1.679(13) . ?
Cl5 C42 1.748(12) . ?
Cl6 C42 1.846(13) . ?
Cl6 Cl6 2.085(12) 2_565 ?
C42 H42 1.0000 . ?
Cl2 C41 1.744(7) . ?
Cl3 C41 1.784(9) . ?
C41 Cl4 1.752(8) . ?
C41 H41 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N1 82.38(19) . . ?
C1 Pd1 N2 167.25(19) . . ?
N1 Pd1 N2 90.44(17) . . ?
C1 Pd1 Cl1 93.17(16) . . ?
N1 Pd1 Cl1 173.29(12) . . ?
N2 Pd1 Cl1 94.83(13) . . ?
C13 N1 C21 119.8(4) . . ?
C13 N1 Pd1 113.5(3) . . ?
C21 N1 Pd1 125.9(3) . . ?
C32 N3 C33 117.8(4) . . ?
C22 N2 C24 117.5(4) . . ?
C22 N2 Pd1 124.7(3) . . ?
C24 N2 Pd1 117.0(3) . . ?
C15 C12 C13 116.6(4) . . ?
C15 C12 C11 125.9(5) . . ?
C13 C12 C11 117.4(4) . . ?
C2 C1 C14 117.1(5) . . ?
C2 C1 Pd1 130.6(4) . . ?
C14 C1 Pd1 112.1(4) . . ?
C10 C11 C6 118.9(5) . . ?
C10 C11 C12 120.7(5) . . ?
C6 C11 C12 120.3(5) . . ?
C27 C28 C29 120.7(6) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C33 C38 C37 118.8(5) . . ?
C33 C38 C39 119.8(5) . . ?
C37 C38 C39 121.3(5) . . ?
C7 C6 C11 118.6(5) . . ?
C7 C6 C5 122.0(5) . . ?
C11 C6 C5 119.3(5) . . ?
N1 C13 C12 123.3(4) . . ?
N1 C13 C14 115.5(4) . . ?
C12 C13 C14 121.1(4) . . ?
C38 C33 C34 121.6(5) . . ?
C38 C33 N3 118.3(5) . . ?
C34 C33 N3 120.0(5) . . ?
C17 C16 C21 119.3(5) . . ?
C17 C16 C15 121.5(5) . . ?
C21 C16 C15 119.3(4) . . ?
C14 C5 C4 116.7(5) . . ?
C14 C5 C6 119.6(5) . . ?
C4 C5 C6 123.7(5) . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C20 C21 117.8(5) . . ?
C19 C20 C22 116.3(5) . . ?
C21 C20 C22 125.7(5) . . ?
C5 C14 C1 124.1(5) . . ?
C5 C14 C13 119.8(5) . . ?
C1 C14 C13 116.1(4) . . ?
C20 C19 C18 122.7(5) . . ?
C20 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
C12 C15 C16 119.4(4) . . ?
C12 C15 C32 118.3(4) . . ?
C16 C15 C32 121.6(4) . . ?
C4 C3 C2 122.2(5) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C2 C1 119.6(5) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C9 C10 C11 121.0(5) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C29 C24 C25 122.1(5) . . ?
C29 C24 N2 120.5(5) . . ?
C25 C24 N2 117.4(5) . . ?
C17 C18 C19 119.8(5) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C35 C34 C33 117.6(5) . . ?
C35 C34 C40 120.1(6) . . ?
C33 C34 C40 122.3(5) . . ?
C24 C29 C28 118.3(5) . . ?
C24 C29 C30 120.9(5) . . ?
C28 C29 C30 120.8(5) . . ?
N2 C22 C20 123.3(5) . . ?
N2 C22 C23 121.1(5) . . ?
C20 C22 C23 115.6(5) . . ?
C8 C7 C6 122.0(5) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C36 C37 C38 120.6(6) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
N1 C21 C16 119.4(4) . . ?
N1 C21 C20 121.5(4) . . ?
C16 C21 C20 119.1(4) . . ?
C3 C4 C5 120.3(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C25 C24 117.6(5) . . ?
C26 C25 C31 121.8(5) . . ?
C24 C25 C31 120.6(5) . . ?
C7 C8 C9 119.9(5) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C26 C25 120.6(5) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C10 C9 C8 119.4(6) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C34 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C36 C35 119.8(6) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C25 C31 H31A 109.5 . . ?
C25 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C36 C35 C34 121.5(6) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N3 C32 C15 124.7(4) . . ?
N3 C32 H32 117.7 . . ?
C15 C32 H32 117.7 . . ?
C42 Cl6 Cl6 168.9(6) . 2_565 ?
Cl7 C42 Cl5 118.7(7) . . ?
Cl7 C42 Cl6 112.8(7) . . ?
Cl5 C42 Cl6 107.8(7) . . ?
Cl7 C42 H42 105.5 . . ?
Cl5 C42 H42 105.5 . . ?
Cl6 C42 H42 105.5 . . ?
Cl2 C41 Cl4 110.4(4) . . ?
Cl2 C41 Cl3 110.6(4) . . ?
Cl4 C41 Cl3 107.6(4) . . ?
Cl2 C41 H41 109.4 . . ?
Cl4 C41 H41 109.4 . . ?
Cl3 C41 H41 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.946
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.238
####################################################################### 
# 
# 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_Pd2
_database_code_depnum_ccdc_archive 'CCDC 1496373'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C44 H40 Cl N3 Pd'
_chemical_formula_sum            'C44 H40 Cl N3 Pd'
_chemical_formula_weight         752.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 'x+2/3, y+1/3, z+1/3'
5 '-y+2/3, x-y+1/3, z+1/3'
6 '-x+y+2/3, -x+1/3, z+1/3'
7 'x+1/3, y+2/3, z+2/3'
8 '-y+1/3, x-y+2/3, z+2/3'
9 '-x+y+1/3, -x+2/3, z+2/3'
10 '-x, -y, -z'
11 'y, -x+y, -z'
12 'x-y, x, -z'
13 '-x+2/3, -y+1/3, -z+1/3'
14 'y+2/3, -x+y+1/3, -z+1/3'
15 'x-y+2/3, x+1/3, -z+1/3'
16 '-x+1/3, -y+2/3, -z+2/3'
17 'y+1/3, -x+y+2/3, -z+2/3'
18 'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   36.490(5)
_cell_length_b                   36.490(5)
_cell_length_c                   21.305(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     24568(7)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    27248
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4384
_cell_measurement_theta_min      1.1161
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.916
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6984
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.306
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            102155
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.12
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 40.1782
	          2theta: -19.9605
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 40.1782
	          2theta: -19.9605
scan:
	Number of images: 330
	           Slice: -110.0000 - 55.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 40.1782
	          2theta: -19.9605
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             12432
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0120
_diffrn_orient_matrix_UB_12      0.0270
_diffrn_orient_matrix_UB_13      -0.0113
_diffrn_orient_matrix_UB_21      -0.0104
_diffrn_orient_matrix_UB_22      0.0278
_diffrn_orient_matrix_UB_23      0.0110
_diffrn_orient_matrix_UB_31      0.0331
_diffrn_orient_matrix_UB_32      -0.0008
_diffrn_orient_matrix_UB_33      0.0333
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                10963
_reflns_number_total             12432
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         12432
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0652
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1448P)²+25.7381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2162
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C42I \\sim C42: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C42I) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(H33C)=Sof(H33D)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C34I)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(H41C)=Sof(H41D)=Sof(C42I)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C41(H41A,H41B), C41(H41C,H41D), C33(H33A,H33B), C33(H33C,
 H33D), C43(H43A,H43B)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C16(H16), C10(H10), C2(H2), C15(H15), C4(H4), C17(H17), C28(H28),
 C9(H9), C7(H7), C39(H39), C8(H8), C3(H3), C26(H26), C38(H38), C37(H37),
 C27(H27)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C44(H44A,H44B,H44C), C42(H42A,H42B,
 H42C), C34I(H34A,H34B,H34C), C34(H34D,H34E,H34F), C42I(H42D,H42E,H42F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pd1 Pd 0.356554(8) 0.239015(8) 0.615104(12) 0.03100(12) Uani 1 d . . . .
N1 N 0.40159(8) 0.24549(8) 0.67697(12) 0.0286(5) Uani 1 d . . . .
Cl1 Cl 0.30131(3) 0.22372(3) 0.54799(5) 0.0461(2) Uani 1 d . . . .
C20 C 0.41372(10) 0.21643(10) 0.66846(15) 0.0298(6) Uani 1 d . . . .
N3 N 0.48420(9) 0.23456(9) 0.86742(14) 0.0350(6) Uani 1 d . . . .
N2 N 0.36858(9) 0.30031(9) 0.63899(15) 0.0357(6) Uani 1 d . . . .
C14 C 0.43545(10) 0.26192(10) 0.77783(15) 0.0289(6) Uani 1 d . . . .
C1 C 0.35916(11) 0.18815(11) 0.58878(17) 0.0360(7) Uani 1 d . . . .
C13 C 0.44874(10) 0.23081(10) 0.76836(15) 0.0302(6) Uani 1 d . . . .
C19 C 0.41414(10) 0.27022(10) 0.72913(15) 0.0290(6) Uani 1 d . . . .
C35 C 0.48841(12) 0.21219(11) 0.91939(17) 0.0377(8) Uani 1 d . . . .
C32 C 0.46159(10) 0.21299(10) 0.82105(16) 0.0321(7) Uani 1 d . . . .
H32 H 0.4526 0.1842 0.8202 0.038 Uiso 1 calc . . R .
C12 C 0.44147(10) 0.21217(10) 0.70991(16) 0.0307(7) Uani 1 d . . . .
C16 C 0.43095(12) 0.31313(11) 0.84452(17) 0.0389(8) Uani 1 d . . . .
H16 H 0.4348 0.3263 0.8833 0.047 Uiso 1 calc . . R .
C11 C 0.45884(11) 0.18526(11) 0.68764(17) 0.0347(7) Uani 1 d . . . .
C22 C 0.39040(10) 0.32221(11) 0.68606(17) 0.0335(7) Uani 1 d . . . .
C10 C 0.49692(12) 0.19081(12) 0.71283(18) 0.0389(8) Uani 1 d . . . .
H10 H 0.5100 0.2099 0.7455 0.047 Uiso 1 calc . . R .
C5 C 0.40358(12) 0.15522(11) 0.60575(17) 0.0374(8) Uani 1 d . . . .
C2 C 0.33545(13) 0.15720(12) 0.54350(17) 0.0402(8) Uani 1 d . . . .
H2 H 0.3134 0.1577 0.5224 0.048 Uiso 1 calc . . R .
C15 C 0.44303(12) 0.28378(11) 0.83625(17) 0.0394(8) Uani 1 d . . . .
H15 H 0.4563 0.2779 0.8688 0.047 Uiso 1 calc . . R .
C40 C 0.52679(12) 0.21246(12) 0.92869(18) 0.0415(8) Uani 1 d A . . .
C18 C 0.40451(10) 0.30390(10) 0.73699(16) 0.0321(7) Uani 1 d . . . .
C4 C 0.37810(14) 0.12425(12) 0.5605(2) 0.0498(10) Uani 1 d . . . .
H4 H 0.3836 0.1026 0.5509 0.060 Uiso 1 calc . . R .
C17 C 0.41271(12) 0.32374(11) 0.79498(18) 0.0388(8) Uani 1 d . . . .
H17 H 0.4059 0.3448 0.8012 0.047 Uiso 1 calc . . R .
C29 C 0.32248(12) 0.32531(12) 0.59600(19) 0.0415(8) Uani 1 d . . . .
C30 C 0.29374(13) 0.30558(14) 0.6512(2) 0.0473(9) Uani 1 d . . . .
H30A H 0.3104 0.3165 0.6891 0.057 Uiso 1 calc . . R .
H30B H 0.2832 0.2754 0.6501 0.057 Uiso 1 calc . . R .
C23 C 0.40259(13) 0.36848(11) 0.6937(2) 0.0446(9) Uani 1 d . . . .
H23A H 0.4011 0.3798 0.6537 0.067 Uiso 1 calc . . GR .
H23B H 0.4309 0.3843 0.7097 0.067 Uiso 1 calc . . GR .
H23C H 0.3834 0.3705 0.7225 0.067 Uiso 1 calc . . GR .
C6 C 0.44034(12) 0.15750(12) 0.63657(18) 0.0399(8) Uani 1 d . . . .
C28 C 0.31456(15) 0.34698(16) 0.5482(2) 0.0550(11) Uani 1 d . . . .
H28 H 0.2912 0.3507 0.5511 0.066 Uiso 1 calc . . R .
C25 C 0.38522(12) 0.33674(13) 0.53699(18) 0.0415(8) Uani 1 d B . . .
C41 C 0.56313(15) 0.23431(17) 0.8838(2) 0.0599(12) Uani 1 d . . . .
H41A H 0.5528 0.2369 0.8431 0.072 Uiso 0.59(4) calc A 1 R .
H41B H 0.5770 0.2178 0.8788 0.072 Uiso 0.59(4) calc A 1 R .
H41C H 0.5559 0.2497 0.8539 0.072 Uiso 0.41(4) calc A 2 R .
H41D H 0.5653 0.2126 0.8606 0.072 Uiso 0.41(4) calc A 2 R .
C24 C 0.35908(11) 0.32196(11) 0.58972(17) 0.0365(7) Uani 1 d . . . .
C9 C 0.51536(14) 0.16802(14) 0.68953(19) 0.0492(10) Uani 1 d . . . .
H9 H 0.5406 0.1719 0.7062 0.059 Uiso 1 calc . . R .
C21 C 0.39262(11) 0.18635(11) 0.61828(16) 0.0334(7) Uani 1 d . . . .
C33 C 0.42279(14) 0.33068(16) 0.5305(2) 0.0542(10) Uani 1 d . . . .
H33A H 0.4371 0.3367 0.5707 0.065 Uiso 0.537(11) calc B 1 R .
H33B H 0.4127 0.3012 0.5209 0.065 Uiso 0.537(11) calc B 1 R .
H33C H 0.4271 0.3191 0.5690 0.065 Uiso 0.463(11) calc B 2 R .
H33D H 0.4481 0.3576 0.5221 0.065 Uiso 0.463(11) calc B 2 R .
C7 C 0.45882(14) 0.13402(13) 0.61535(19) 0.0471(9) Uani 1 d . . . .
H7 H 0.4459 0.1145 0.5832 0.057 Uiso 1 calc . . R .
C39 C 0.53041(14) 0.19244(13) 0.9837(2) 0.0527(10) Uani 1 d . . . .
H39 H 0.5552 0.1918 0.9908 0.063 Uiso 1 calc A . R .
C8 C 0.49525(14) 0.13936(14) 0.6410(2) 0.0502(10) Uani 1 d . . . .
H8 H 0.5070 0.1236 0.6258 0.060 Uiso 1 calc . . R .
C3 C 0.34538(14) 0.12583(12) 0.53057(19) 0.0476(9) Uani 1 d . . . .
H3 H 0.3295 0.1053 0.5009 0.057 Uiso 1 calc . . R .
C31 C 0.25579(15) 0.31239(17) 0.6560(2) 0.0607(12) Uani 1 d . . . .
H31A H 0.2375 0.2996 0.6205 0.091 Uiso 1 calc . . GR .
H31B H 0.2655 0.3422 0.6565 0.091 Uiso 1 calc . . GR .
H31C H 0.2405 0.2997 0.6939 0.091 Uiso 1 calc . . GR .
C36 C 0.45477(13) 0.19253(12) 0.96321(18) 0.0432(8) Uani 1 d A . . .
C26 C 0.37600(16) 0.35779(17) 0.4915(2) 0.0618(12) Uani 1 d . . . .
H26 H 0.3936 0.3687 0.4567 0.074 Uiso 1 calc B . R .
C38 C 0.49877(16) 0.17441(16) 1.0256(2) 0.0608(12) Uani 1 d A . . .
H38 H 0.5020 0.1615 1.0611 0.073 Uiso 1 calc . . R .
C37 C 0.46067(16) 0.17482(15) 1.0166(2) 0.0576(11) Uani 1 d . . . .
H37 H 0.4395 0.1631 1.0468 0.069 Uiso 1 calc A . R .
C43 C 0.41337(15) 0.19308(16) 0.9522(2) 0.0612(12) Uani 1 d . . . .
H43A H 0.4207 0.2211 0.9378 0.073 Uiso 1 calc A . R .
H43B H 0.3981 0.1735 0.9184 0.073 Uiso 1 calc . . R .
C27 C 0.34142(17) 0.36291(18) 0.4966(2) 0.0657(13) Uani 1 d B . . .
H27 H 0.3358 0.3772 0.4653 0.079 Uiso 1 calc . . R .
C44 C 0.38400(18) 0.18216(18) 1.0068(3) 0.0758(15) Uani 1 d A . . .
H44A H 0.3608 0.1862 0.9954 0.114 Uiso 1 calc . . GR .
H44B H 0.3989 0.2001 1.0416 0.114 Uiso 1 calc . . GR .
H44C H 0.3734 0.1531 1.0184 0.114 Uiso 1 calc . . GR .
C42 C 0.5943(5) 0.2778(5) 0.9088(6) 0.073(4) Uani 0.59(4) d A 1 . U
H42A H 0.5805 0.2942 0.9131 0.110 Uiso 0.59(4) calc A 1 GR .
H42B H 0.6176 0.2917 0.8801 0.110 Uiso 0.59(4) calc A 1 GR .
H42C H 0.6047 0.2751 0.9490 0.110 Uiso 0.59(4) calc A 1 GR .
C34I C 0.4543(3) 0.3572(4) 0.4819(6) 0.093(4) Uani 0.537(11) d B 1 . .
H34A H 0.4434 0.3459 0.4410 0.139 Uiso 0.537(11) calc B 1 GR .
H34B H 0.4802 0.3570 0.4887 0.139 Uiso 0.537(11) calc B 1 GR .
H34C H 0.4595 0.3857 0.4845 0.139 Uiso 0.537(11) calc B 1 GR .
C34 C 0.4137(3) 0.2987(4) 0.4735(5) 0.060(3) Uani 0.463(11) d B 2 . .
H34D H 0.3928 0.2706 0.4861 0.091 Uiso 0.463(11) calc B 2 GR .
H34E H 0.4393 0.2992 0.4622 0.091 Uiso 0.463(11) calc B 2 GR .
H34F H 0.4033 0.3072 0.4382 0.091 Uiso 0.463(11) calc B 2 GR .
C42I C 0.6063(6) 0.2646(8) 0.9095(8) 0.067(6) Uani 0.41(4) d A 2 . U
H42D H 0.6046 0.2667 0.9542 0.100 Uiso 0.41(4) calc A 2 GR .
H42E H 0.6166 0.2919 0.8909 0.100 Uiso 0.41(4) calc A 2 GR .
H42F H 0.6254 0.2544 0.8997 0.100 Uiso 0.41(4) calc A 2 GR .


_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 N1 2.026(3) . ?
Pd1 Cl1 2.3010(9) . ?
Pd1 N2 2.115(3) . ?
Pd1 C1 1.986(3) . ?
N1 C20 1.350(4) . ?
N1 C19 1.359(4) . ?
C20 C12 1.409(4) . ?
C20 C21 1.447(4) . ?
N3 C35 1.429(4) . ?
N3 C32 1.275(4) . ?
N2 C22 1.281(4) . ?
N2 C24 1.456(4) . ?
C14 C13 1.454(4) . ?
C14 C19 1.417(4) . ?
C14 C15 1.429(5) . ?
C1 C2 1.406(5) . ?
C1 C21 1.403(5) . ?
C13 C32 1.486(4) . ?
C13 C12 1.380(5) . ?
C19 C18 1.447(4) . ?
C35 C40 1.410(5) . ?
C35 C36 1.419(5) . ?
C32 H32 0.9300 . ?
C12 C11 1.488(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.358(5) . ?
C16 C17 1.402(5) . ?
C11 C10 1.407(5) . ?
C11 C6 1.408(5) . ?
C22 C18 1.494(5) . ?
C22 C23 1.524(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.397(5) . ?
C5 C4 1.422(5) . ?
C5 C6 1.458(5) . ?
C5 C21 1.406(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(5) . ?
C15 H15 0.9300 . ?
C40 C41 1.500(6) . ?
C40 C39 1.422(5) . ?
C18 C17 1.387(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.380(6) . ?
C17 H17 0.9300 . ?
C29 C30 1.498(6) . ?
C29 C28 1.405(5) . ?
C29 C24 1.407(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.528(6) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C6 C7 1.404(5) . ?
C28 H28 0.9300 . ?
C28 C27 1.392(7) . ?
C25 C24 1.396(5) . ?
C25 C33 1.500(6) . ?
C25 C26 1.378(6) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C41 H41D 0.9700 . ?
C41 C42 1.513(13) . ?
C41 C42I 1.504(16) . ?
C9 H9 0.9300 . ?
C9 C8 1.391(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C33 H33D 0.9700 . ?
C33 C34I 1.489(12) . ?
C33 C34 1.599(11) . ?
C7 H7 0.9300 . ?
C7 C8 1.358(6) . ?
C39 H39 0.9300 . ?
C39 C38 1.343(7) . ?
C8 H8 0.9300 . ?
C3 H3 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C36 C37 1.377(6) . ?
C36 C43 1.539(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.369(7) . ?
C38 H38 0.9300 . ?
C38 C37 1.411(7) . ?
C37 H37 0.9300 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.494(7) . ?
C27 H27 0.9300 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C34I H34A 0.9600 . ?
C34I H34B 0.9600 . ?
C34I H34C 0.9600 . ?
C34 H34D 0.9600 . ?
C34 H34E 0.9600 . ?
C34 H34F 0.9600 . ?
C42I H42D 0.9600 . ?
C42I H42E 0.9600 . ?
C42I H42F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 Cl1 173.53(8) . . ?
N1 Pd1 N2 89.59(10) . . ?
N2 Pd1 Cl1 95.71(8) . . ?
C1 Pd1 N1 82.98(12) . . ?
C1 Pd1 Cl1 92.48(11) . . ?
C1 Pd1 N2 167.08(13) . . ?
C20 N1 Pd1 112.7(2) . . ?
C20 N1 C19 119.8(3) . . ?
C19 N1 Pd1 126.4(2) . . ?
N1 C20 C12 122.6(3) . . ?
N1 C20 C21 115.8(3) . . ?
C12 C20 C21 121.2(3) . . ?
C32 N3 C35 117.9(3) . . ?
C22 N2 Pd1 125.7(2) . . ?
C22 N2 C24 117.9(3) . . ?
C24 N2 Pd1 114.9(2) . . ?
C19 C14 C13 119.9(3) . . ?
C19 C14 C15 119.5(3) . . ?
C15 C14 C13 120.6(3) . . ?
C2 C1 Pd1 130.3(3) . . ?
C21 C1 Pd1 111.5(2) . . ?
C21 C1 C2 118.0(3) . . ?
C14 C13 C32 122.6(3) . . ?
C12 C13 C14 116.9(3) . . ?
C12 C13 C32 119.4(3) . . ?
N1 C19 C14 119.7(3) . . ?
N1 C19 C18 121.0(3) . . ?
C14 C19 C18 119.3(3) . . ?
C40 C35 N3 119.7(3) . . ?
C40 C35 C36 121.1(3) . . ?
C36 C35 N3 119.1(3) . . ?
N3 C32 C13 124.3(3) . . ?
N3 C32 H32 117.9 . . ?
C13 C32 H32 117.9 . . ?
C20 C12 C11 116.1(3) . . ?
C13 C12 C20 118.9(3) . . ?
C13 C12 C11 125.0(3) . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C6 118.8(3) . . ?
C6 C11 C12 120.8(3) . . ?
N2 C22 C18 122.3(3) . . ?
N2 C22 C23 121.4(3) . . ?
C18 C22 C23 116.3(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 C11 120.9(4) . . ?
C9 C10 H10 119.5 . . ?
C4 C5 C6 124.6(3) . . ?
C21 C5 C4 115.7(3) . . ?
C21 C5 C6 119.6(3) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.8 . . ?
C35 C40 C41 121.7(3) . . ?
C35 C40 C39 117.4(4) . . ?
C39 C40 C41 120.9(4) . . ?
C19 C18 C22 125.5(3) . . ?
C17 C18 C19 117.8(3) . . ?
C17 C18 C22 116.5(3) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4 119.5 . . ?
C16 C17 H17 118.8 . . ?
C18 C17 C16 122.3(3) . . ?
C18 C17 H17 118.8 . . ?
C28 C29 C30 123.2(4) . . ?
C28 C29 C24 116.8(4) . . ?
C24 C29 C30 120.0(3) . . ?
C29 C30 H30A 108.1 . . ?
C29 C30 H30B 108.1 . . ?
C29 C30 C31 116.6(4) . . ?
H30A C30 H30B 107.3 . . ?
C31 C30 H30A 108.1 . . ?
C31 C30 H30B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C11 C6 C5 119.1(3) . . ?
C7 C6 C11 119.0(3) . . ?
C7 C6 C5 121.9(4) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 C29 120.5(4) . . ?
C27 C28 H28 119.8 . . ?
C24 C25 C33 121.0(3) . . ?
C26 C25 C24 118.1(4) . . ?
C26 C25 C33 120.9(4) . . ?
C40 C41 H41A 109.7 . . ?
C40 C41 H41B 109.7 . . ?
C40 C41 H41C 107.6 . . ?
C40 C41 H41D 107.6 . . ?
C40 C41 C42 109.6(7) . . ?
C40 C41 C42I 118.9(7) . . ?
H41A C41 H41B 108.2 . . ?
H41A C41 H41C 28.7 . . ?
H41A C41 H41D 79.4 . . ?
H41B C41 H41C 131.9 . . ?
H41B C41 H41D 32.3 . . ?
H41C C41 H41D 107.0 . . ?
C42 C41 H41A 109.7 . . ?
C42 C41 H41B 109.7 . . ?
C42 C41 H41C 84.4 . . ?
C42 C41 H41D 135.2 . . ?
C42I C41 H41A 124.8 . . ?
C42I C41 H41B 79.3 . . ?
C42I C41 H41C 107.6 . . ?
C42I C41 H41D 107.6 . . ?
C42I C41 C42 30.7(7) . . ?
C29 C24 N2 118.2(3) . . ?
C25 C24 N2 119.2(3) . . ?
C25 C24 C29 122.6(3) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 H9 120.6 . . ?
C1 C21 C20 116.2(3) . . ?
C1 C21 C5 123.9(3) . . ?
C5 C21 C20 119.6(3) . . ?
C25 C33 H33A 108.4 . . ?
C25 C33 H33B 108.4 . . ?
C25 C33 H33C 110.2 . . ?
C25 C33 H33D 110.2 . . ?
C25 C33 C34 107.8(5) . . ?
H33A C33 H33B 107.4 . . ?
H33A C33 H33C 33.4 . . ?
H33A C33 H33D 78.6 . . ?
H33B C33 H33C 75.5 . . ?
H33B C33 H33D 136.6 . . ?
H33C C33 H33D 108.5 . . ?
C34I C33 C25 115.7(6) . . ?
C34I C33 H33A 108.4 . . ?
C34I C33 H33B 108.4 . . ?
C34I C33 H33C 129.1 . . ?
C34I C33 H33D 35.0 . . ?
C34I C33 C34 75.9(7) . . ?
C34 C33 H33A 136.6 . . ?
C34 C33 H33B 37.3 . . ?
C34 C33 H33C 110.2 . . ?
C34 C33 H33D 110.2 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(4) . . ?
C8 C7 H7 119.4 . . ?
C40 C39 H39 119.3 . . ?
C38 C39 C40 121.5(4) . . ?
C38 C39 H39 119.3 . . ?
C9 C8 H8 119.4 . . ?
C7 C8 C9 121.1(4) . . ?
C7 C8 H8 119.4 . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.0(3) . . ?
C4 C3 H3 119.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C35 C36 C43 120.0(3) . . ?
C37 C36 C35 118.8(4) . . ?
C37 C36 C43 121.1(4) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 C25 121.3(5) . . ?
C27 C26 H26 119.4 . . ?
C39 C38 H38 119.5 . . ?
C39 C38 C37 120.9(4) . . ?
C37 C38 H38 119.5 . . ?
C36 C37 C38 120.2(4) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C36 C43 H43A 108.0 . . ?
C36 C43 H43B 108.0 . . ?
H43A C43 H43B 107.3 . . ?
C44 C43 C36 117.1(4) . . ?
C44 C43 H43A 108.0 . . ?
C44 C43 H43B 108.0 . . ?
C28 C27 H27 119.7 . . ?
C26 C27 C28 120.7(4) . . ?
C26 C27 H27 119.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
C33 C34I H34A 109.5 . . ?
C33 C34I H34B 109.5 . . ?
C33 C34I H34C 109.5 . . ?
C33 C34 H34D 109.5 . . ?
C33 C34 H34E 109.5 . . ?
C33 C34 H34F 109.5 . . ?
H34D C34 H34E 109.5 . . ?
H34D C34 H34F 109.5 . . ?
H34E C34 H34F 109.5 . . ?
C41 C42I H42D 109.5 . . ?
C41 C42I H42E 109.5 . . ?
C41 C42I H42F 109.5 . . ?
H42D C42I H42E 109.5 . . ?
H42D C42I H42F 109.5 . . ?
H42E C42I H42F 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
Pd1 N1 C20 C12 -173.4(3) . . . . ?
Pd1 N1 C20 C21 -0.5(4) . . . . ?
Pd1 N1 C19 C14 160.0(2) . . . . ?
Pd1 N1 C19 C18 -17.4(4) . . . . ?
Pd1 N2 C22 C18 -10.5(5) . . . . ?
Pd1 N2 C22 C23 170.9(3) . . . . ?
Pd1 N2 C24 C29 105.4(3) . . . . ?
Pd1 N2 C24 C25 -71.6(4) . . . . ?
Pd1 C1 C2 C3 175.6(3) . . . . ?
Pd1 C1 C21 C20 9.9(4) . . . . ?
Pd1 C1 C21 C5 -176.1(3) . . . . ?
N1 Pd1 N2 C22 -12.6(3) . . . . ?
N1 Pd1 N2 C24 152.9(2) . . . . ?
N1 Pd1 C1 C2 177.4(4) . . . . ?
N1 Pd1 C1 C21 -7.9(3) . . . . ?
N1 C20 C12 C13 15.7(5) . . . . ?
N1 C20 C12 C11 -167.8(3) . . . . ?
N1 C20 C21 C1 -6.3(5) . . . . ?
N1 C20 C21 C5 179.4(3) . . . . ?
N1 C19 C18 C22 -15.7(5) . . . . ?
N1 C19 C18 C17 170.7(3) . . . . ?
Cl1 Pd1 N1 C20 50.3(8) . . . . ?
Cl1 Pd1 N1 C19 -118.1(7) . . . . ?
Cl1 Pd1 N2 C22 163.7(3) . . . . ?
Cl1 Pd1 N2 C24 -30.8(2) . . . . ?
Cl1 Pd1 C1 C2 2.1(4) . . . . ?
Cl1 Pd1 C1 C21 176.8(3) . . . . ?
C20 N1 C19 C14 -7.7(5) . . . . ?
C20 N1 C19 C18 174.9(3) . . . . ?
C20 C12 C11 C10 157.0(3) . . . . ?
C20 C12 C11 C6 -15.8(5) . . . . ?
N3 C35 C40 C41 -2.4(6) . . . . ?
N3 C35 C40 C39 175.3(3) . . . . ?
N3 C35 C36 C37 -173.3(4) . . . . ?
N3 C35 C36 C43 3.8(5) . . . . ?
N2 Pd1 N1 C20 -164.7(2) . . . . ?
N2 Pd1 N1 C19 26.8(3) . . . . ?
N2 Pd1 C1 C2 -127.3(6) . . . . ?
N2 Pd1 C1 C21 47.4(7) . . . . ?
N2 C22 C18 C19 30.8(5) . . . . ?
N2 C22 C18 C17 -155.6(4) . . . . ?
C14 C13 C32 N3 -40.8(5) . . . . ?
C14 C13 C12 C20 -14.4(5) . . . . ?
C14 C13 C12 C11 169.4(3) . . . . ?
C14 C19 C18 C22 166.9(3) . . . . ?
C14 C19 C18 C17 -6.7(5) . . . . ?
C1 Pd1 N1 C20 4.7(2) . . . . ?
C1 Pd1 N1 C19 -163.8(3) . . . . ?
C1 Pd1 N2 C22 -67.3(7) . . . . ?
C1 Pd1 N2 C24 98.3(6) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C13 C14 C19 N1 8.2(5) . . . . ?
C13 C14 C19 C18 -174.4(3) . . . . ?
C13 C14 C15 C16 179.3(3) . . . . ?
C13 C12 C11 C10 -26.7(5) . . . . ?
C13 C12 C11 C6 160.5(3) . . . . ?
C19 N1 C20 C12 -4.1(5) . . . . ?
C19 N1 C20 C21 168.8(3) . . . . ?
C19 C14 C13 C32 -164.9(3) . . . . ?
C19 C14 C13 C12 3.1(5) . . . . ?
C19 C14 C15 C16 -1.8(5) . . . . ?
C19 C18 C17 C16 2.0(5) . . . . ?
C35 N3 C32 C13 170.1(3) . . . . ?
C35 C40 C41 C42 97.5(10) . . . . ?
C35 C40 C41 C42I 129.7(15) . . . . ?
C35 C40 C39 C38 -0.8(6) . . . . ?
C35 C36 C37 C38 -3.3(7) . . . . ?
C35 C36 C43 C44 -164.6(4) . . . . ?
C32 N3 C35 C40 106.3(4) . . . . ?
C32 N3 C35 C36 -78.1(4) . . . . ?
C32 C13 C12 C20 154.0(3) . . . . ?
C32 C13 C12 C11 -22.2(5) . . . . ?
C12 C20 C21 C1 166.6(3) . . . . ?
C12 C20 C21 C5 -7.6(5) . . . . ?
C12 C13 C32 N3 151.5(3) . . . . ?
C12 C11 C10 C9 -175.4(3) . . . . ?
C12 C11 C6 C5 -0.3(5) . . . . ?
C12 C11 C6 C7 177.3(4) . . . . ?
C11 C10 C9 C8 -0.4(6) . . . . ?
C11 C6 C7 C8 -3.6(6) . . . . ?
C22 N2 C24 C29 -87.9(4) . . . . ?
C22 N2 C24 C25 95.1(4) . . . . ?
C22 C18 C17 C16 -172.1(3) . . . . ?
C10 C11 C6 C5 -173.1(3) . . . . ?
C10 C11 C6 C7 4.5(6) . . . . ?
C10 C9 C8 C7 1.4(6) . . . . ?
C5 C4 C3 C2 -0.7(7) . . . . ?
C5 C6 C7 C8 174.0(4) . . . . ?
C2 C1 C21 C20 -174.7(3) . . . . ?
C2 C1 C21 C5 -0.7(6) . . . . ?
C15 C14 C13 C32 14.1(5) . . . . ?
C15 C14 C13 C12 -177.9(3) . . . . ?
C15 C14 C19 N1 -170.8(3) . . . . ?
C15 C14 C19 C18 6.6(5) . . . . ?
C15 C16 C17 C18 2.9(6) . . . . ?
C40 C35 C36 C37 2.3(6) . . . . ?
C40 C35 C36 C43 179.4(4) . . . . ?
C40 C39 C38 C37 -0.2(7) . . . . ?
C4 C5 C6 C11 -169.9(4) . . . . ?
C4 C5 C6 C7 12.6(6) . . . . ?
C4 C5 C21 C20 173.3(4) . . . . ?
C4 C5 C21 C1 -0.5(6) . . . . ?
C17 C16 C15 C14 -3.0(6) . . . . ?
C29 C28 C27 C26 0.0(8) . . . . ?
C30 C29 C28 C27 -177.0(4) . . . . ?
C30 C29 C24 N2 -2.1(5) . . . . ?
C30 C29 C24 C25 174.8(4) . . . . ?
C23 C22 C18 C19 -150.5(3) . . . . ?
C23 C22 C18 C17 23.1(5) . . . . ?
C6 C11 C10 C9 -2.6(6) . . . . ?
C6 C5 C4 C3 -175.9(4) . . . . ?
C6 C5 C21 C20 -9.5(5) . . . . ?
C6 C5 C21 C1 176.7(4) . . . . ?
C6 C7 C8 C9 0.6(7) . . . . ?
C28 C29 C30 C31 -3.8(6) . . . . ?
C28 C29 C24 N2 179.0(3) . . . . ?
C28 C29 C24 C25 -4.1(6) . . . . ?
C25 C26 C27 C28 0.1(8) . . . . ?
C41 C40 C39 C38 177.0(4) . . . . ?
C24 N2 C22 C18 -175.6(3) . . . . ?
C24 N2 C22 C23 5.7(5) . . . . ?
C24 C29 C30 C31 177.3(4) . . . . ?
C24 C29 C28 C27 2.0(7) . . . . ?
C24 C25 C33 C34I -164.4(7) . . . . ?
C24 C25 C33 C34 113.0(6) . . . . ?
C24 C25 C26 C27 -2.2(7) . . . . ?
C21 C20 C12 C13 -156.8(3) . . . . ?
C21 C20 C12 C11 19.7(5) . . . . ?
C21 C1 C2 C3 1.2(6) . . . . ?
C21 C5 C4 C3 1.1(6) . . . . ?
C21 C5 C6 C11 13.2(5) . . . . ?
C21 C5 C6 C7 -164.4(4) . . . . ?
C33 C25 C24 N2 -0.1(5) . . . . ?
C33 C25 C24 C29 -176.9(4) . . . . ?
C33 C25 C26 C27 179.0(5) . . . . ?
C39 C40 C41 C42 -80.2(10) . . . . ?
C39 C40 C41 C42I -48.0(15) . . . . ?
C39 C38 C37 C36 2.3(8) . . . . ?
C36 C35 C40 C41 -178.0(4) . . . . ?
C36 C35 C40 C39 -0.3(5) . . . . ?
C26 C25 C24 N2 -178.9(4) . . . . ?
C26 C25 C24 C29 4.3(6) . . . . ?
C26 C25 C33 C34I 14.3(9) . . . . ?
C26 C25 C33 C34 -68.2(7) . . . . ?
C37 C36 C43 C44 12.5(7) . . . . ?
C43 C36 C37 C38 179.6(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          
;
;
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
_platon_squeeze_void_content
1 -0.012 -0.009 0.000 10078 4649 ' '
####################################################################### 
# 
# 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_Pd3
_database_code_depnum_ccdc_archive 'CCDC 1496374'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_audit_creation_date             2016-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H23 Cl N2 O Pd, C H2 Cl2'
_chemical_formula_sum            'C33 H25 Cl3 N2 O Pd'
_chemical_formula_weight         678.30
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.611(2)
_cell_length_b                   19.188(4)
_cell_length_c                   13.466(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.15(3)
_cell_angle_gamma                90.00
_cell_volume                     2758.5(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8526
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4848
_cell_measurement_theta_min      1.6455
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7964
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368.0
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.128
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19114
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.24
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0951
	          2theta: -20.0130
scan:
	Number of images: 298
	           Slice: -80.0000 - 69.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0951
	          2theta: -20.0130
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_number_total             6451
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0853
_diffrn_orient_matrix_UB_12      -0.0094
_diffrn_orient_matrix_UB_13      -0.0375
_diffrn_orient_matrix_UB_21      -0.0070
_diffrn_orient_matrix_UB_22      -0.0515
_diffrn_orient_matrix_UB_23      -0.0030
_diffrn_orient_matrix_UB_31      -0.0000
_diffrn_orient_matrix_UB_32      0.0048
_diffrn_orient_matrix_UB_33      -0.0807
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5993
_reflns_number_total             6237
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0299P)²+4.5904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0850
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C8(H8), C3(H3), C26(H26), C10(H10), C7(H7), C4(H4), C2(H2),
 C28(H28), C27(H27), C9(H9), C16(H16), C17(H17), C15(H15)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.214174(18) 0.422474(10) 0.430988(14) 0.02090(7) Uani 1 d . . .
Cl1 Cl 0.25353(7) 0.31171(3) 0.38610(5) 0.03046(15) Uani 1 d . . .
C12 C 0.1789(2) 0.57535(13) 0.6434(2) 0.0221(5) Uani 1 d . . .
N1 N 0.16896(19) 0.51408(11) 0.48151(16) 0.0206(4) Uani 1 d . . .
C18 C 0.0723(2) 0.56880(14) 0.3018(2) 0.0238(5) Uani 1 d . . .
C11 C 0.2358(2) 0.57566(14) 0.7624(2) 0.0247(5) Uani 1 d . . .
N2 N 0.1778(2) 0.46389(11) 0.27629(16) 0.0228(4) Uani 1 d . . .
O1 O 0.0727(3) 0.74836(12) 0.60771(18) 0.0470(6) Uani 1 d . . .
C19 C 0.1035(2) 0.56763(13) 0.41692(19) 0.0209(5) Uani 1 d . . .
C1 C 0.2682(2) 0.39726(14) 0.5851(2) 0.0245(5) Uani 1 d . . .
C14 C 0.0635(2) 0.62425(13) 0.4647(2) 0.0234(5) Uani 1 d . . .
C21 C 0.2562(2) 0.45377(13) 0.6475(2) 0.0233(5) Uani 1 d . . .
C32 C 0.0607(3) 0.68791(16) 0.6259(2) 0.0316(6) Uani 1 d . . .
H32 H 0.0215 0.6777 0.6726 0.038 Uiso 1 calc . . R
C13 C 0.1047(2) 0.62811(13) 0.5785(2) 0.0234(5) Uani 1 d . . .
C24 C 0.2314(3) 0.42571(13) 0.2118(2) 0.0241(5) Uani 1 d . . .
C20 C 0.2005(2) 0.51647(13) 0.58969(19) 0.0210(5) Uani 1 d . . .
C8 C 0.3382(3) 0.57424(18) 0.9891(2) 0.0367(7) Uani 1 d . . .
H8 H 0.3681 0.5733 1.0641 0.044 Uiso 1 calc . . R
C3 C 0.3590(3) 0.33158(16) 0.7515(2) 0.0354(7) Uani 1 d . . .
H3 H 0.3935 0.2902 0.7865 0.042 Uiso 1 calc . . R
C22 C 0.1258(2) 0.52335(14) 0.2414(2) 0.0252(5) Uani 1 d . . .
C5 C 0.2933(2) 0.45015(15) 0.7599(2) 0.0261(5) Uani 1 d . . .
C6 C 0.2845(2) 0.51277(15) 0.8189(2) 0.0260(5) Uani 1 d . . .
C25 C 0.1551(3) 0.37988(14) 0.1325(2) 0.0264(5) Uani 1 d . . .
C26 C 0.2095(3) 0.34322(15) 0.0728(2) 0.0322(6) Uani 1 d . . .
H26 H 0.1606 0.3132 0.0184 0.039 Uiso 1 calc . . R
C10 C 0.2495(3) 0.63726(16) 0.8224(2) 0.0316(6) Uani 1 d . . .
H10 H 0.2243 0.6794 0.7862 0.038 Uiso 1 calc . . R
C7 C 0.3320(3) 0.51373(17) 0.9325(2) 0.0333(6) Uani 1 d . . .
H7 H 0.3599 0.4723 0.9703 0.040 Uiso 1 calc . . R
C4 C 0.3456(3) 0.38699(16) 0.8108(2) 0.0330(6) Uani 1 d . . .
H4 H 0.3713 0.3827 0.8852 0.040 Uiso 1 calc . . R
C23 C 0.1176(3) 0.55172(16) 0.1336(2) 0.0355(7) Uani 1 d . . .
H23A H 0.0330 0.5477 0.0814 0.053 Uiso 1 calc . . GR
H23B H 0.1723 0.5256 0.1096 0.053 Uiso 1 calc . . GR
H23C H 0.1422 0.5998 0.1416 0.053 Uiso 1 calc . . GR
C29 C 0.3578(3) 0.43474(15) 0.2335(2) 0.0297(6) Uani 1 d . . .
C2 C 0.3218(3) 0.33634(15) 0.6392(2) 0.0298(6) Uani 1 d . . .
H2 H 0.3330 0.2985 0.6008 0.036 Uiso 1 calc . . R
C28 C 0.4090(3) 0.39596(16) 0.1732(3) 0.0365(7) Uani 1 d . . .
H28 H 0.4936 0.4005 0.1870 0.044 Uiso 1 calc . . R
C27 C 0.3356(3) 0.35097(16) 0.0935(3) 0.0374(7) Uani 1 d . . .
H27 H 0.3708 0.3258 0.0534 0.045 Uiso 1 calc . . R
C9 C 0.2995(3) 0.63669(18) 0.9339(2) 0.0371(7) Uani 1 d . . .
H9 H 0.3073 0.6781 0.9719 0.044 Uiso 1 calc . . R
C16 C -0.0543(3) 0.67337(15) 0.2884(2) 0.0299(6) Uani 1 d . . .
H16 H -0.1096 0.7065 0.2448 0.036 Uiso 1 calc . . R
C17 C -0.0075(3) 0.62105(15) 0.2425(2) 0.0293(6) Uani 1 d . . .
H17 H -0.0313 0.6213 0.1680 0.035 Uiso 1 calc . . R
C15 C -0.0185(3) 0.67562(14) 0.3971(2) 0.0273(5) Uani 1 d . . .
H15 H -0.0479 0.7112 0.4279 0.033 Uiso 1 calc . . R
C31 C 0.0210(3) 0.36871(16) 0.1158(2) 0.0321(6) Uani 1 d . . .
H31A H 0.0174 0.3428 0.1755 0.048 Uiso 1 calc . . GR
H31B H -0.0211 0.3432 0.0501 0.048 Uiso 1 calc . . GR
H31C H -0.0193 0.4130 0.1111 0.048 Uiso 1 calc . . GR
C30 C 0.4371(3) 0.48443(18) 0.3194(3) 0.0417(7) Uani 1 d . . .
H30A H 0.4163 0.5315 0.2944 0.062 Uiso 1 calc . . GR
H30B H 0.5240 0.4760 0.3349 0.062 Uiso 1 calc . . GR
H30C H 0.4217 0.4776 0.3838 0.062 Uiso 1 calc . . GR
Cl2 Cl 0.38425(11) 0.81757(7) 1.06406(12) 0.0835(4) Uani 1 d . . .
Cl3 Cl 0.33458(13) 0.81990(6) 0.83352(12) 0.0856(4) Uani 1 d . . .
C33 C 0.4301(5) 0.8429(4) 0.9624(5) 0.127(3) Uani 1 d . . .
H33A H 0.4385 0.8933 0.9650 0.152 Uiso 1 calc . . R
H33B H 0.5126 0.8236 0.9778 0.152 Uiso 1 calc . . R


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.3039(8) . ?
Pd1 N1 2.027(2) . ?
Pd1 N2 2.111(2) . ?
Pd1 C1 1.978(3) . ?
C12 C11 1.473(3) . ?
C12 C13 1.393(4) . ?
C12 C20 1.416(4) . ?
N1 C19 1.368(3) . ?
N1 C20 1.356(3) . ?
C18 C19 1.447(3) . ?
C18 C22 1.486(4) . ?
C18 C17 1.386(4) . ?
C11 C6 1.420(4) . ?
C11 C10 1.406(4) . ?
N2 C24 1.450(3) . ?
N2 C22 1.290(3) . ?
O1 C32 1.205(4) . ?
C19 C14 1.430(4) . ?
C1 C21 1.412(4) . ?
C1 C2 1.388(4) . ?
C14 C13 1.416(3) . ?
C14 C15 1.423(4) . ?
C21 C20 1.441(3) . ?
C21 C5 1.404(3) . ?
C32 C13 1.498(4) . ?
C24 C25 1.398(4) . ?
C24 C29 1.390(4) . ?
C8 C7 1.375(4) . ?
C8 C9 1.388(5) . ?
C3 C4 1.375(4) . ?
C3 C2 1.402(4) . ?
C22 C23 1.517(4) . ?
C5 C6 1.466(4) . ?
C5 C4 1.407(4) . ?
C6 C7 1.408(4) . ?
C25 C26 1.393(4) . ?
C25 C31 1.499(4) . ?
C26 C27 1.386(5) . ?
C10 C9 1.380(4) . ?
C29 C28 1.395(4) . ?
C29 C30 1.502(4) . ?
C28 C27 1.380(5) . ?
C16 C17 1.396(4) . ?
C16 C15 1.356(4) . ?
Cl2 C33 1.723(7) . ?
Cl3 C33 1.710(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 Cl1 172.84(6) . . ?
N1 Pd1 N2 91.55(8) . . ?
N2 Pd1 Cl1 94.11(6) . . ?
C1 Pd1 Cl1 92.05(8) . . ?
C1 Pd1 N1 82.94(10) . . ?
C1 Pd1 N2 170.18(10) . . ?
C13 C12 C11 125.6(2) . . ?
C13 C12 C20 116.7(2) . . ?
C20 C12 C11 117.7(2) . . ?
C19 N1 Pd1 126.20(16) . . ?
C20 N1 Pd1 113.19(16) . . ?
C20 N1 C19 120.4(2) . . ?
C19 C18 C22 126.6(2) . . ?
C17 C18 C19 117.2(2) . . ?
C17 C18 C22 116.0(2) . . ?
C6 C11 C12 119.6(2) . . ?
C10 C11 C12 122.0(2) . . ?
C10 C11 C6 118.4(2) . . ?
C24 N2 Pd1 115.74(16) . . ?
C22 N2 Pd1 125.17(18) . . ?
C22 N2 C24 118.5(2) . . ?
N1 C19 C18 122.4(2) . . ?
N1 C19 C14 118.8(2) . . ?
C14 C19 C18 118.8(2) . . ?
C21 C1 Pd1 111.82(18) . . ?
C2 C1 Pd1 130.4(2) . . ?
C2 C1 C21 117.6(2) . . ?
C13 C14 C19 119.7(2) . . ?
C13 C14 C15 120.8(2) . . ?
C15 C14 C19 119.5(2) . . ?
C1 C21 C20 116.6(2) . . ?
C5 C21 C1 122.9(2) . . ?
C5 C21 C20 120.4(2) . . ?
O1 C32 C13 124.4(3) . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 C32 121.3(2) . . ?
C14 C13 C32 118.4(2) . . ?
C25 C24 N2 118.9(2) . . ?
C29 C24 N2 118.5(2) . . ?
C29 C24 C25 122.6(3) . . ?
C12 C20 C21 121.5(2) . . ?
N1 C20 C12 123.3(2) . . ?
N1 C20 C21 115.2(2) . . ?
C7 C8 C9 119.8(3) . . ?
C4 C3 C2 121.2(3) . . ?
C18 C22 C23 115.5(2) . . ?
N2 C22 C18 123.8(2) . . ?
N2 C22 C23 120.7(2) . . ?
C21 C5 C6 119.1(2) . . ?
C21 C5 C4 117.3(3) . . ?
C4 C5 C6 123.4(2) . . ?
C11 C6 C5 120.3(2) . . ?
C7 C6 C11 118.3(3) . . ?
C7 C6 C5 121.2(3) . . ?
C24 C25 C31 120.9(2) . . ?
C26 C25 C24 117.7(3) . . ?
C26 C25 C31 121.4(3) . . ?
C27 C26 C25 120.8(3) . . ?
C9 C10 C11 121.6(3) . . ?
C8 C7 C6 121.7(3) . . ?
C3 C4 C5 120.6(3) . . ?
C24 C29 C28 117.9(3) . . ?
C24 C29 C30 121.2(3) . . ?
C28 C29 C30 120.9(3) . . ?
C1 C2 C3 120.4(3) . . ?
C27 C28 C29 120.9(3) . . ?
C28 C27 C26 120.2(3) . . ?
C10 C9 C8 119.9(3) . . ?
C15 C16 C17 119.6(2) . . ?
C18 C17 C16 123.6(2) . . ?
C16 C15 C14 120.8(3) . . ?
Cl3 C33 Cl2 117.0(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Pd4
_database_code_depnum_ccdc_archive 'CCDC 1496375'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C34 H27 Cl N2 O Pd'
_chemical_formula_sum            'C34 H27 Cl N2 O Pd'
_chemical_formula_weight         621.43
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.187(3)
_cell_length_b                   12.380(3)
_cell_length_c                   14.674(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.59(3)
_cell_angle_gamma                90.00
_cell_volume                     2574.7(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4793
_cell_measurement_theta_min      1.3892
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.119
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32464
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.95
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 40.0117
	          2theta: -20.9371
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 40.0117
	          2theta: -20.9371
scan:
	Number of images: 328
	           Slice: -110.0000 - 54.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 40.0117
	          2theta: -20.9371
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             6179
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0555
_diffrn_orient_matrix_UB_12      0.0426
_diffrn_orient_matrix_UB_13      -0.0091
_diffrn_orient_matrix_UB_21      0.0020
_diffrn_orient_matrix_UB_22      -0.0143
_diffrn_orient_matrix_UB_23      -0.0795
_diffrn_orient_matrix_UB_31      -0.0445
_diffrn_orient_matrix_UB_32      -0.0511
_diffrn_orient_matrix_UB_33      0.0081
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5816
_reflns_number_total             5894
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5894
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0330P)²+2.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0708
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C32(H32), C17(H17), C15(H15), C27(H27), C8(H8), C16(H16), C10(H10),
 C9(H9), C2(H2), C4(H4), C7(H7), C28(H28), C3(H3)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.537490(9) 0.446921(10) 0.274700(9) 0.01644(6) Uani 1 d . . .
Cl1 Cl 0.41827(3) 0.39294(4) 0.17306(3) 0.02634(11) Uani 1 d . . .
O1 O 0.81914(11) 0.55244(11) 0.68069(10) 0.0269(3) Uani 1 d . . .
N2 N 0.63922(11) 0.33840(12) 0.22451(10) 0.0189(3) Uani 1 d . . .
C30 C 0.65641(15) 0.49537(16) 0.07777(14) 0.0273(4) Uani 1 d . . .
H30A H 0.6335 0.5198 0.1371 0.033 Uiso 1 calc . . R
H30B H 0.6273 0.5421 0.0295 0.033 Uiso 1 calc . . R
C22 C 0.71887(13) 0.31630(15) 0.26526(13) 0.0205(4) Uani 1 d . . .
C26 C 0.57576(14) 0.16570(17) 0.02412(14) 0.0267(4) Uani 1 d . . .
H26 H 0.5601 0.0926 0.0107 0.032 Uiso 1 calc . . R
C32 C 0.74054(14) 0.56707(15) 0.64816(13) 0.0199(4) Uani 1 d . . .
H32 H 0.6944 0.5932 0.6876 0.024 Uiso 1 calc . . R
C14 C 0.74016(13) 0.45275(13) 0.50426(12) 0.0171(3) Uani 1 d . . .
C18 C 0.74052(13) 0.34273(14) 0.36308(12) 0.0193(3) Uani 1 d . . .
C17 C 0.80873(14) 0.27909(15) 0.40741(13) 0.0226(4) Uani 1 d . . .
H17 H 0.8364 0.2224 0.3741 0.027 Uiso 1 calc . . R
N1 N 0.62661(10) 0.48949(12) 0.38034(10) 0.0164(3) Uani 1 d . . .
C15 C 0.80677(13) 0.38050(15) 0.54543(13) 0.0208(4) Uani 1 d . . .
H15 H 0.8293 0.3925 0.6065 0.025 Uiso 1 calc . . R
C27 C 0.57854(15) 0.24013(18) -0.04650(14) 0.0277(4) Uani 1 d . . .
H27 H 0.5641 0.2181 -0.1075 0.033 Uiso 1 calc . . R
C29 C 0.62557(13) 0.37988(15) 0.06102(13) 0.0218(4) Uani 1 d . . .
C8 C 0.55695(15) 0.91929(16) 0.61274(14) 0.0257(4) Uani 1 d . . .
H8 H 0.5358 0.9847 0.6387 0.031 Uiso 1 calc . . R
C16 C 0.83894(13) 0.29406(15) 0.49864(13) 0.0226(4) Uani 1 d . . .
H16 H 0.8815 0.2443 0.5277 0.027 Uiso 1 calc . . R
C13 C 0.70991(13) 0.54728(14) 0.55030(12) 0.0173(3) Uani 1 d . . .
C12 C 0.64325(12) 0.61519(14) 0.50797(12) 0.0163(3) Uani 1 d . . .
C19 C 0.70106(13) 0.42962(14) 0.41432(12) 0.0165(3) Uani 1 d . . .
C23 C 0.79734(15) 0.26044(18) 0.21579(14) 0.0290(4) Uani 1 d . . .
H23A H 0.7983 0.1835 0.2313 0.044 Uiso 1 calc . . GR
H23B H 0.8581 0.2931 0.2344 0.044 Uiso 1 calc . . GR
H23C H 0.7861 0.2689 0.1498 0.044 Uiso 1 calc . . GR
C10 C 0.67178(14) 0.77805(15) 0.60649(13) 0.0219(4) Uani 1 d . . .
H10 H 0.7315 0.7493 0.6257 0.026 Uiso 1 calc . . R
C21 C 0.51091(12) 0.62584(14) 0.39100(12) 0.0167(3) Uani 1 d . . .
C34 C 0.54918(16) 0.00819(17) 0.16926(17) 0.0333(5) Uani 1 d . . .
H34A H 0.5897 -0.0260 0.1252 0.050 Uiso 1 calc . . GR
H34B H 0.4849 0.0147 0.1424 0.050 Uiso 1 calc . . GR
H34C H 0.5484 -0.0361 0.2246 0.050 Uiso 1 calc . . GR
C20 C 0.59669(12) 0.57631(14) 0.42669(12) 0.0159(3) Uani 1 d . . .
C9 C 0.64311(15) 0.87543(16) 0.64194(14) 0.0252(4) Uani 1 d . . .
H9 H 0.6822 0.9122 0.6861 0.030 Uiso 1 calc . . R
C2 C 0.38271(13) 0.62042(15) 0.27941(12) 0.0207(4) Uani 1 d . . .
H2 H 0.3504 0.5885 0.2281 0.025 Uiso 1 calc . . R
C4 C 0.39153(13) 0.76321(15) 0.39279(13) 0.0224(4) Uani 1 d . . .
H4 H 0.3652 0.8263 0.4183 0.027 Uiso 1 calc . . R
C7 C 0.50203(14) 0.86777(16) 0.54594(14) 0.0244(4) Uani 1 d . . .
H7 H 0.4442 0.8998 0.5249 0.029 Uiso 1 calc . . R
C11 C 0.61453(13) 0.72071(14) 0.54262(12) 0.0178(3) Uani 1 d . . .
C1 C 0.46476(13) 0.57334(15) 0.31580(12) 0.0183(3) Uani 1 d . . .
C28 C 0.60233(15) 0.34616(18) -0.02786(14) 0.0271(4) Uani 1 d . . .
H28 H 0.6029 0.3970 -0.0763 0.033 Uiso 1 calc . . R
C3 C 0.34733(13) 0.71454(16) 0.31788(13) 0.0230(4) Uani 1 d . . .
H3 H 0.2913 0.7459 0.2917 0.028 Uiso 1 calc . . R
C24 C 0.62182(13) 0.30402(15) 0.13074(12) 0.0200(4) Uani 1 d . . .
C33 C 0.5869(2) 0.11888(18) 0.19318(16) 0.0414(6) Uani 1 d . . .
H33A H 0.6500 0.1104 0.2239 0.050 Uiso 1 calc . . R
H33B H 0.5452 0.1520 0.2377 0.050 Uiso 1 calc . . R
C5 C 0.47561(13) 0.71947(14) 0.43146(12) 0.0186(3) Uani 1 d . . .
C25 C 0.59556(14) 0.19630(16) 0.11436(13) 0.0239(4) Uani 1 d . . .
C6 C 0.52978(13) 0.76894(15) 0.50843(12) 0.0194(3) Uani 1 d . . .
C31 C 0.76315(19) 0.5079(2) 0.0785(2) 0.0514(7) Uani 1 d . . .
H31A H 0.7861 0.4842 0.0198 0.077 Uiso 1 calc . . GR
H31B H 0.7922 0.4637 0.1275 0.077 Uiso 1 calc . . GR
H31C H 0.7799 0.5839 0.0887 0.077 Uiso 1 calc . . GR


_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 2.3030(8) . ?
Pd1 N2 2.1276(16) . ?
Pd1 N1 2.0254(16) . ?
Pd1 C1 1.9834(19) . ?
O1 C32 1.207(2) . ?
N2 C22 1.284(2) . ?
N2 C24 1.451(2) . ?
C30 C29 1.512(3) . ?
C30 C31 1.522(3) . ?
C22 C18 1.491(3) . ?
C22 C23 1.522(3) . ?
C26 C27 1.389(3) . ?
C26 C25 1.394(3) . ?
C32 C13 1.501(3) . ?
C14 C15 1.416(3) . ?
C14 C13 1.427(2) . ?
C14 C19 1.437(3) . ?
C18 C17 1.387(3) . ?
C18 C19 1.440(2) . ?
C17 C16 1.399(3) . ?
N1 C19 1.366(2) . ?
N1 C20 1.351(2) . ?
C15 C16 1.361(3) . ?
C27 C28 1.380(3) . ?
C29 C28 1.395(3) . ?
C29 C24 1.392(3) . ?
C8 C9 1.387(3) . ?
C8 C7 1.381(3) . ?
C13 C12 1.391(2) . ?
C12 C20 1.421(2) . ?
C12 C11 1.466(2) . ?
C10 C9 1.381(3) . ?
C10 C11 1.405(3) . ?
C21 C20 1.440(2) . ?
C21 C1 1.416(2) . ?
C21 C5 1.405(2) . ?
C34 C33 1.507(3) . ?
C2 C1 1.387(3) . ?
C2 C3 1.398(3) . ?
C4 C3 1.379(3) . ?
C4 C5 1.406(3) . ?
C7 C6 1.405(3) . ?
C11 C6 1.414(3) . ?
C24 C25 1.403(3) . ?
C33 C25 1.511(3) . ?
C5 C6 1.471(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 Cl1 94.73(5) . . ?
N1 Pd1 Cl1 170.39(4) . . ?
N1 Pd1 N2 91.11(6) . . ?
C1 Pd1 Cl1 92.80(6) . . ?
C1 Pd1 N2 166.88(7) . . ?
C1 Pd1 N1 82.95(7) . . ?
C22 N2 Pd1 124.75(13) . . ?
C22 N2 C24 119.19(16) . . ?
C24 N2 Pd1 115.12(12) . . ?
C29 C30 C31 112.22(18) . . ?
N2 C22 C18 122.71(17) . . ?
N2 C22 C23 121.46(17) . . ?
C18 C22 C23 115.82(17) . . ?
C27 C26 C25 121.16(19) . . ?
O1 C32 C13 125.18(18) . . ?
C15 C14 C13 121.68(17) . . ?
C15 C14 C19 119.22(16) . . ?
C13 C14 C19 119.09(16) . . ?
C17 C18 C22 115.85(17) . . ?
C17 C18 C19 117.32(17) . . ?
C19 C18 C22 126.77(16) . . ?
C18 C17 C16 123.40(18) . . ?
C19 N1 Pd1 125.72(12) . . ?
C20 N1 Pd1 113.14(12) . . ?
C20 N1 C19 120.23(15) . . ?
C16 C15 C14 120.92(17) . . ?
C28 C27 C26 119.89(18) . . ?
C28 C29 C30 119.30(18) . . ?
C24 C29 C30 122.63(17) . . ?
C24 C29 C28 118.04(18) . . ?
C7 C8 C9 119.97(18) . . ?
C15 C16 C17 119.43(17) . . ?
C14 C13 C32 120.42(16) . . ?
C12 C13 C32 119.35(16) . . ?
C12 C13 C14 119.82(17) . . ?
C13 C12 C20 116.82(16) . . ?
C13 C12 C11 125.29(16) . . ?
C20 C12 C11 117.83(16) . . ?
C14 C19 C18 119.03(16) . . ?
N1 C19 C14 119.15(16) . . ?
N1 C19 C18 121.81(16) . . ?
C9 C10 C11 121.40(18) . . ?
C1 C21 C20 116.20(16) . . ?
C5 C21 C20 120.61(16) . . ?
C5 C21 C1 123.17(16) . . ?
N1 C20 C12 123.19(16) . . ?
N1 C20 C21 115.81(15) . . ?
C12 C20 C21 120.94(16) . . ?
C10 C9 C8 119.70(18) . . ?
C1 C2 C3 120.35(17) . . ?
C3 C4 C5 120.02(18) . . ?
C8 C7 C6 121.41(18) . . ?
C10 C11 C12 121.35(17) . . ?
C10 C11 C6 118.69(17) . . ?
C6 C11 C12 119.89(16) . . ?
C21 C1 Pd1 111.76(13) . . ?
C2 C1 Pd1 130.82(14) . . ?
C2 C1 C21 117.24(17) . . ?
C27 C28 C29 121.03(19) . . ?
C4 C3 C2 121.83(17) . . ?
C29 C24 N2 119.26(16) . . ?
C29 C24 C25 122.31(17) . . ?
C25 C24 N2 118.29(17) . . ?
C34 C33 C25 116.02(19) . . ?
C21 C5 C4 117.34(17) . . ?
C21 C5 C6 118.96(16) . . ?
C4 C5 C6 123.64(17) . . ?
C26 C25 C24 117.51(18) . . ?
C26 C25 C33 122.34(18) . . ?
C24 C25 C33 120.13(17) . . ?
C7 C6 C11 118.53(17) . . ?
C7 C6 C5 121.16(17) . . ?
C11 C6 C5 120.21(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_L1
_database_code_depnum_ccdc_archive 'CCDC 1496529'
_audit_update_record             
;
2016-07-28 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H33 N3 O0'
_chemical_formula_weight         555.69

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.910(2)
_cell_length_b                   32.793(7)
_cell_length_c                   9.4655(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.37(3)
_cell_angle_gamma                90.00
_cell_volume                     3393.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9817
_cell_measurement_theta_min      1.8631
_cell_measurement_theta_max      27.4851

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9857
_exptl_absorpt_correction_T_max  0.9936

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23288
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7780
_reflns_number_gt                6204
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0528P)²+1.2942P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7780
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1406
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001

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
N1 N 0.50060(13) 0.14548(4) 0.45846(16) 0.0295(3) Uani 1 1 d . . .
C15 C 0.63445(15) 0.21782(5) 0.48448(18) 0.0270(3) Uani 1 1 d . . .
C16 C 0.66883(15) 0.18148(5) 0.42822(18) 0.0281(3) Uani 1 1 d . . .
N3 N 0.49391(14) 0.05761(4) 0.19361(18) 0.0363(3) Uani 1 1 d . . .
C12 C 0.46851(15) 0.17968(5) 0.50688(18) 0.0279(3) Uani 1 1 d . . .
C13 C 0.52645(15) 0.21809(5) 0.51004(18) 0.0281(3) Uani 1 1 d . . .
C14 C 0.47020(15) 0.25511(5) 0.53963(19) 0.0307(4) Uani 1 1 d . . .
C32 C 0.72066(15) 0.25246(5) 0.53899(19) 0.0284(3) Uani 1 1 d . . .
H32 H 0.7253 0.2661 0.6296 0.034 Uiso 1 1 calc R . .
N2 N 0.78913(13) 0.26541(4) 0.47399(16) 0.0312(3) Uani 1 1 d . . .
C6 C 0.33024(15) 0.21188(5) 0.61497(19) 0.0329(4) Uani 1 1 d . . .
C11 C 0.37239(15) 0.17665(5) 0.56650(19) 0.0312(4) Uani 1 1 d . . .
C21 C 0.59476(15) 0.14620(5) 0.41266(18) 0.0281(3) Uani 1 1 d . . .
C1 C 0.50132(16) 0.29415(5) 0.5044(2) 0.0356(4) Uani 1 1 d . . .
H1 H 0.5596 0.2965 0.4595 0.043 Uiso 1 1 calc R . .
C5 C 0.37601(15) 0.25210(5) 0.59439(19) 0.0332(4) Uani 1 1 d . . .
C33 C 0.87820(15) 0.29562(5) 0.55234(19) 0.0288(3) Uani 1 1 d . . .
C34 C 0.97644(15) 0.28619(5) 0.69090(19) 0.0303(4) Uani 1 1 d . . .
C7 C 0.24090(17) 0.20724(6) 0.6760(2) 0.0416(4) Uani 1 1 d . . .
H7 H 0.2112 0.2306 0.7096 0.050 Uiso 1 1 calc R . .
C38 C 0.87045(16) 0.33343(5) 0.4799(2) 0.0338(4) Uani 1 1 d . . .
C17 C 0.77069(16) 0.17819(5) 0.3869(2) 0.0324(4) Uani 1 1 d . . .
H17 H 0.8256 0.2005 0.4051 0.039 Uiso 1 1 calc R . .
C19 C 0.71366(17) 0.10944(5) 0.2989(2) 0.0376(4) Uani 1 1 d . . .
H19 H 0.7274 0.0858 0.2500 0.045 Uiso 1 1 calc R . .
C29 C 0.48740(19) -0.01657(5) 0.1705(2) 0.0395(4) Uani 1 1 d . . .
C18 C 0.79070(17) 0.14334(5) 0.3214(2) 0.0371(4) Uani 1 1 d . . .
H18 H 0.8575 0.1420 0.2907 0.045 Uiso 1 1 calc R . .
C22 C 0.54289(17) 0.07250(5) 0.3284(2) 0.0338(4) Uani 1 1 d . . .
C10 C 0.32475(17) 0.13831(6) 0.5794(2) 0.0390(4) Uani 1 1 d . . .
H10 H 0.3531 0.1146 0.5462 0.047 Uiso 1 1 calc R . .
C20 C 0.61905(16) 0.10991(5) 0.34613(19) 0.0313(4) Uani 1 1 d . . .
C3 C 0.36181(18) 0.32590(6) 0.5945(2) 0.0443(5) Uani 1 1 d . . .
H3 H 0.3274 0.3498 0.6176 0.053 Uiso 1 1 calc R . .
C35 C 1.06565(16) 0.31582(6) 0.7559(2) 0.0381(4) Uani 1 1 d . . .
H35 H 1.1326 0.3102 0.8502 0.046 Uiso 1 1 calc R . .
C24 C 0.42674(18) 0.02031(5) 0.1652(2) 0.0380(4) Uani 1 1 d . . .
C2 C 0.44928(18) 0.32916(6) 0.5333(2) 0.0420(5) Uani 1 1 d . . .
H2 H 0.4734 0.3552 0.5114 0.050 Uiso 1 1 calc R . .
C37 C 0.96231(18) 0.36190(5) 0.5499(2) 0.0394(4) Uani 1 1 d . . .
H37 H 0.9582 0.3877 0.5027 0.047 Uiso 1 1 calc R . .
C8 C 0.19577(18) 0.16933(7) 0.6879(2) 0.0470(5) Uani 1 1 d . . .
H8 H 0.1355 0.1669 0.7296 0.056 Uiso 1 1 calc R . .
C36 C 1.05921(17) 0.35329(6) 0.6865(2) 0.0411(4) Uani 1 1 d . . .
H36 H 1.1213 0.3731 0.7328 0.049 Uiso 1 1 calc R . .
C40 C 0.98807(17) 0.24521(5) 0.7684(2) 0.0378(4) Uani 1 1 d . . .
H40A H 0.9274 0.2431 0.8139 0.057 Uiso 1 1 calc R . .
H40B H 1.0704 0.2424 0.8493 0.057 Uiso 1 1 calc R . .
H40C H 0.9740 0.2235 0.6921 0.057 Uiso 1 1 calc R . .
C9 C 0.23724(18) 0.13478(6) 0.6398(3) 0.0474(5) Uani 1 1 d . . .
H9 H 0.2055 0.1087 0.6483 0.057 Uiso 1 1 calc R . .
C4 C 0.32433(17) 0.28815(6) 0.6221(2) 0.0403(4) Uani 1 1 d . . .
H4 H 0.2621 0.2864 0.6608 0.048 Uiso 1 1 calc R . .
C30 C 0.6235(2) -0.01826(6) 0.2260(3) 0.0518(5) Uani 1 1 d . . .
H30A H 0.6520 0.0042 0.1805 0.078 Uiso 1 1 calc R . .
H30B H 0.6477 -0.0443 0.1955 0.078 Uiso 1 1 calc R . .
H30C H 0.6602 -0.0159 0.3384 0.078 Uiso 1 1 calc R . .
C28 C 0.4167(2) -0.05167(6) 0.1205(2) 0.0478(5) Uani 1 1 d . . .
H28 H 0.4560 -0.0770 0.1226 0.057 Uiso 1 1 calc R . .
C25 C 0.2997(2) 0.02197(6) 0.1136(3) 0.0499(5) Uani 1 1 d . . .
C26 C 0.2334(2) -0.01407(7) 0.0681(3) 0.0603(6) Uani 1 1 d . . .
H26 H 0.1470 -0.0136 0.0363 0.072 Uiso 1 1 calc R . .
C39 C 0.7640(2) 0.34269(6) 0.3316(2) 0.0517(5) Uani 1 1 d . . .
H39A H 0.7496 0.3195 0.2613 0.078 Uiso 1 1 calc R . .
H39B H 0.7821 0.3670 0.2844 0.078 Uiso 1 1 calc R . .
H39C H 0.6908 0.3476 0.3525 0.078 Uiso 1 1 calc R . .
C27 C 0.2916(2) -0.05048(6) 0.0685(3) 0.0566(6) Uani 1 1 d . . .
H27 H 0.2451 -0.0747 0.0328 0.068 Uiso 1 1 calc R . .
C23 C 0.5395(2) 0.05357(5) 0.4713(2) 0.0490(5) Uani 1 1 d . . .
H23A H 0.4575 0.0428 0.4487 0.074 Uiso 1 1 calc R . .
H23B H 0.5597 0.0742 0.5524 0.074 Uiso 1 1 calc R . .
H23C H 0.5993 0.0313 0.5059 0.074 Uiso 1 1 calc R . .
C31 C 0.2367(2) 0.06196(7) 0.1080(4) 0.0766(8) Uani 1 1 d . . .
H31A H 0.2468 0.0796 0.0302 0.115 Uiso 1 1 calc R . .
H31B H 0.2728 0.0752 0.2089 0.115 Uiso 1 1 calc R . .
H31C H 0.1494 0.0572 0.0812 0.115 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C12 1.324(2) . ?
N1 C21 1.353(2) . ?
C15 C13 1.400(2) . ?
C15 C16 1.430(2) . ?
C15 C32 1.480(2) . ?
C16 C17 1.419(2) . ?
C16 C21 1.427(2) . ?
N3 C22 1.271(2) . ?
N3 C24 1.427(2) . ?
C12 C13 1.431(2) . ?
C12 C11 1.467(2) . ?
C13 C14 1.466(2) . ?
C14 C1 1.409(2) . ?
C14 C5 1.414(2) . ?
C32 N2 1.274(2) . ?
N2 C33 1.426(2) . ?
C6 C7 1.406(2) . ?
C6 C11 1.407(2) . ?
C6 C5 1.469(2) . ?
C11 C10 1.405(2) . ?
C21 C20 1.429(2) . ?
C1 C2 1.383(2) . ?
C5 C4 1.405(2) . ?
C33 C38 1.402(2) . ?
C33 C34 1.403(2) . ?
C34 C35 1.390(2) . ?
C34 C40 1.511(2) . ?
C7 C8 1.376(3) . ?
C38 C37 1.390(2) . ?
C38 C39 1.503(3) . ?
C17 C18 1.366(2) . ?
C19 C20 1.368(2) . ?
C19 C18 1.403(2) . ?
C29 C28 1.393(3) . ?
C29 C24 1.400(2) . ?
C29 C30 1.494(3) . ?
C22 C20 1.495(2) . ?
C22 C23 1.503(2) . ?
C10 C9 1.378(3) . ?
C3 C4 1.376(3) . ?
C3 C2 1.382(3) . ?
C35 C36 1.381(3) . ?
C24 C25 1.394(3) . ?
C37 C36 1.379(3) . ?
C8 C9 1.383(3) . ?
C28 C27 1.371(3) . ?
C25 C26 1.392(3) . ?
C25 C31 1.502(3) . ?
C26 C27 1.380(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
C12 N1 C21 119.07(14) . . ?
C13 C15 C16 119.21(14) . . ?
C13 C15 C32 119.52(14) . . ?
C16 C15 C32 120.53(14) . . ?
C17 C16 C21 118.11(14) . . ?
C17 C16 C15 124.66(15) . . ?
C21 C16 C15 117.24(15) . . ?
C22 N3 C24 121.21(15) . . ?
N1 C12 C13 123.35(15) . . ?
N1 C12 C11 116.91(14) . . ?
C13 C12 C11 119.67(14) . . ?
C15 C13 C12 117.35(14) . . ?
C15 C13 C14 123.98(15) . . ?
C12 C13 C14 118.68(15) . . ?
C1 C14 C5 118.16(15) . . ?
C1 C14 C13 121.60(16) . . ?
C5 C14 C13 120.08(15) . . ?
N2 C32 C15 125.18(15) . . ?
C32 N2 C33 117.86(14) . . ?
C7 C6 C11 118.11(16) . . ?
C7 C6 C5 122.19(16) . . ?
C11 C6 C5 119.64(15) . . ?
C10 C11 C6 119.86(16) . . ?
C10 C11 C12 119.86(15) . . ?
C6 C11 C12 120.26(15) . . ?
N1 C21 C16 122.54(14) . . ?
N1 C21 C20 117.72(14) . . ?
C16 C21 C20 119.74(15) . . ?
C2 C1 C14 121.78(18) . . ?
C4 C5 C14 118.68(17) . . ?
C4 C5 C6 121.17(17) . . ?
C14 C5 C6 120.10(15) . . ?
C38 C33 C34 121.38(15) . . ?
C38 C33 N2 117.98(15) . . ?
C34 C33 N2 120.39(15) . . ?
C35 C34 C33 117.86(16) . . ?
C35 C34 C40 120.01(16) . . ?
C33 C34 C40 122.12(15) . . ?
C8 C7 C6 121.00(18) . . ?
C37 C38 C33 118.32(16) . . ?
C37 C38 C39 121.50(16) . . ?
C33 C38 C39 120.18(15) . . ?
C18 C17 C16 120.76(16) . . ?
C20 C19 C18 121.03(16) . . ?
C28 C29 C24 117.88(19) . . ?
C28 C29 C30 120.95(18) . . ?
C24 C29 C30 121.16(17) . . ?
C17 C18 C19 120.70(16) . . ?
N3 C22 C20 116.38(15) . . ?
N3 C22 C23 125.38(16) . . ?
C20 C22 C23 118.00(16) . . ?
C9 C10 C11 120.63(18) . . ?
C19 C20 C21 119.40(15) . . ?
C19 C20 C22 119.73(15) . . ?
C21 C20 C22 120.87(15) . . ?
C4 C3 C2 120.30(17) . . ?
C36 C35 C34 121.54(17) . . ?
C25 C24 C29 121.28(17) . . ?
C25 C24 N3 118.80(16) . . ?
C29 C24 N3 119.41(17) . . ?
C3 C2 C1 119.35(18) . . ?
C36 C37 C38 121.15(17) . . ?
C7 C8 C9 120.71(18) . . ?
C37 C36 C35 119.75(17) . . ?
C10 C9 C8 119.69(19) . . ?
C3 C4 C5 121.50(18) . . ?
C27 C28 C29 121.51(19) . . ?
C26 C25 C24 118.65(19) . . ?
C26 C25 C31 121.1(2) . . ?
C24 C25 C31 120.27(18) . . ?
C27 C26 C25 120.7(2) . . ?
C28 C27 C26 119.92(19) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.040
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 0.000 0.500 0.000 302.0 62.0
2 0.000 1.000 0.500 302.1 62.0
_platon_squeeze_details          
; ?
;
