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

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

data_79cv92
_database_code_depnum_ccdc_archive 'CCDC 1493764'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-03-23
_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         'C25 H32 Br2 N4 Pd'
_chemical_formula_sum            'C25 H32 Br2 N4 Pd'
_chemical_formula_weight         654.77
_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'
Br Br -0.2901 2.4595 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x, y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z-1/2'
8 'x, -y-1/2, z'

_cell_length_a                   12.691(2)
_cell_length_b                   26.883(2)
_cell_length_c                   7.540(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2572.4(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19504
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      3.03
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27427
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.03
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3374
_reflns_number_total             3822
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.318
_refine_diff_density_min         -2.190
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0528
_refine_ls_restrained_S_all      1.059
_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)+(0.0659P)²+8.9852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1399
_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:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.21292(3) 0.2500 0.14520(5) 0.02415(12) Uani 1 d . . 2 S T P
Br1 Br 0.29874(3) 0.31432(2) -0.04078(5) 0.03935(15) Uani 1 d . . 1 . . .
N1 N 0.1040(3) 0.34545(13) 0.2803(4) 0.0288(6) Uani 1 d . . 1 . . .
N2 N 0.1545(3) 0.29404(13) 0.4827(4) 0.0275(6) Uani 1 d . . 1 . . .
C1 C 0.1520(3) 0.30206(14) 0.3077(5) 0.0249(7) Uani 1 d . . 1 . . .
C2 C 0.0669(4) 0.36859(16) 0.4483(5) 0.0335(8) Uani 1 d . . 1 . . .
H2A H -0.0102 0.3741 0.4459 0.040 Uiso 1 calc . . 1 R . .
H2B H 0.1027 0.4007 0.4699 0.040 Uiso 1 calc . . 1 R . .
C3 C 0.0968(4) 0.33034(18) 0.5885(5) 0.0363(9) Uani 1 d . . 1 . . .
H3A H 0.1419 0.3451 0.6818 0.044 Uiso 1 calc . . 1 R . .
H3B H 0.0336 0.3154 0.6441 0.044 Uiso 1 calc . . 1 R . .
C4 C 0.0867(3) 0.37458(15) 0.1231(5) 0.0306(8) Uani 1 d . . 1 . . .
C5 C -0.0019(3) 0.36532(16) 0.0200(5) 0.0304(7) Uani 1 d . . 1 . . .
C6 C -0.0255(5) 0.39928(19) -0.1145(6) 0.0446(11) Uani 1 d . . 1 . . .
H6 H -0.0859 0.3940 -0.1865 0.053 Uiso 1 calc . . 1 R . .
C7 C 0.0380(7) 0.44089(19) -0.1452(7) 0.0619(18) Uani 1 d . . 1 . . .
C8 C 0.1260(7) 0.4478(2) -0.0416(7) 0.0656(19) Uani 1 d . . 1 . . .
H8 H 0.1702 0.4755 -0.0650 0.079 Uiso 1 calc . . 1 R . .
C9 C 0.1527(5) 0.41583(19) 0.0958(7) 0.0510(13) Uani 1 d . . 1 . . .
C10 C -0.0688(4) 0.3211(2) 0.0484(6) 0.0414(10) Uani 1 d . . 1 . . .
H10A H -0.0276 0.2909 0.0255 0.062 Uiso 1 calc . . 1 GR . .
H10B H -0.1291 0.3222 -0.0326 0.062 Uiso 1 calc . . 1 GR . .
H10C H -0.0941 0.3207 0.1712 0.062 Uiso 1 calc . . 1 GR . .
C11 C 0.0094(10) 0.4778(3) -0.2909(8) 0.097(3) Uani 1 d . . 1 . . .
H11A H 0.0085 0.5116 -0.2418 0.145 Uiso 1 calc . . 1 GR . .
H11B H -0.0604 0.4697 -0.3382 0.145 Uiso 1 calc . . 1 GR . .
H11C H 0.0617 0.4759 -0.3863 0.145 Uiso 1 calc . . 1 GR . .
C12 C 0.2481(6) 0.4256(3) 0.2075(8) 0.0679(19) Uani 1 d . . 1 . . .
H12A H 0.2292 0.4478 0.3056 0.102 Uiso 1 calc . . 1 GR . .
H12B H 0.3028 0.4413 0.1347 0.102 Uiso 1 calc . . 1 GR . .
H12C H 0.2747 0.3941 0.2551 0.102 Uiso 1 calc . . 1 GR . .
C13 C 0.1995(5) 0.2500 0.5587(8) 0.0335(12) Uani 1 d . . 2 S T P
H13A H 0.1872 0.2500 0.6883 0.040 Uiso 1 calc . . 2 RS T P
H13B H 0.2766 0.2500 0.5384 0.040 Uiso 1 calc . . 2 RS T P


_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 Br1 2.4785(6) . ?
Pd1 Br1 2.4785(6) 8_565 ?
Pd1 C1 2.014(4) . ?
Pd1 C1 2.015(4) 8_565 ?
N1 C1 1.332(5) . ?
N1 C2 1.487(5) . ?
N1 C4 1.438(5) . ?
N2 C1 1.337(4) . ?
N2 C3 1.458(5) . ?
N2 C13 1.434(4) . ?
C2 C3 1.523(6) . ?
C4 C5 1.389(6) . ?
C4 C9 1.405(6) . ?
C5 C6 1.398(6) . ?
C5 C10 1.477(6) . ?
C6 C7 1.398(9) . ?
C7 C8 1.374(10) . ?
C7 C11 1.525(8) . ?
C8 C9 1.388(8) . ?
C9 C12 1.498(9) . ?
C13 N2 1.434(4) 8_565 ?

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
Br1 Pd1 Br1 88.48(3) . 8_565 ?
C1 Pd1 Br1 91.61(10) . . ?
C1 Pd1 Br1 175.99(10) 8_565 . ?
C1 Pd1 Br1 91.61(10) 8_565 8_565 ?
C1 Pd1 Br1 175.99(10) . 8_565 ?
C1 Pd1 C1 88.0(2) . 8_565 ?
C1 N1 C2 112.3(3) . . ?
C1 N1 C4 132.4(3) . . ?
C4 N1 C2 115.2(3) . . ?
C1 N2 C3 114.8(3) . . ?
C1 N2 C13 122.5(4) . . ?
C13 N2 C3 122.3(4) . . ?
N1 C1 Pd1 133.6(3) . . ?
N1 C1 N2 107.8(3) . . ?
N2 C1 Pd1 118.6(3) . . ?
N1 C2 C3 103.3(3) . . ?
N2 C3 C2 101.4(3) . . ?
C5 C4 N1 119.1(3) . . ?
C5 C4 C9 122.8(4) . . ?
C9 C4 N1 117.4(4) . . ?
C4 C5 C6 117.6(4) . . ?
C4 C5 C10 121.9(4) . . ?
C6 C5 C10 120.5(4) . . ?
C5 C6 C7 121.2(5) . . ?
C6 C7 C11 120.2(7) . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 C11 121.0(7) . . ?
C7 C8 C9 122.6(5) . . ?
C4 C9 C12 122.5(5) . . ?
C8 C9 C4 116.9(5) . . ?
C8 C9 C12 120.6(5) . . ?
N2 C13 N2 111.3(4) . 8_565 ?

_olex2_submission_original_sample_id as79cv92
_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_74cv79
_database_code_depnum_ccdc_archive 'CCDC 1493769'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-07-15
_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         '2(C27 H36 Ag N4), 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C58 H78 Ag2 F12 N10 P2'
_chemical_formula_weight         1420.98
_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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.142(4)
_cell_length_b                   26.641(2)
_cell_length_c                   15.776(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.79(1)
_cell_angle_gamma                90.00
_cell_volume                     6252(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    69645
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      1.52
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            103477
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.52
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                12688
_reflns_number_total             14918
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.661
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         14918
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0688P)²+10.0380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1189
_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:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C17(H17A,H17B), C18(H18A,H18B), C29(H29A,H29B), C30(H30A,H30B), C40(H40A,H40B),
  C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C21(H21), C23(H23), C33(H33), C35(H35), C48(H48), C50(H50)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C)
;
_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
Ag1 Ag 0.407349(14) 0.561347(8) 0.356438(13) 0.01836(6) Uani 1 d . . .
N1 N 0.25343(17) 0.50221(9) 0.25101(16) 0.0221(5) Uani 1 d . . .
N2 N 0.30397(17) 0.46194(9) 0.36935(15) 0.0211(5) Uani 1 d . . .
N3 N 0.40951(16) 0.38399(9) 0.60871(15) 0.0198(5) Uani 1 d . . .
N4 N 0.52084(17) 0.33253(9) 0.60806(17) 0.0220(5) Uani 1 d . . .
C1 C 0.31387(19) 0.50270(10) 0.32429(18) 0.0189(5) Uani 1 d . . .
C2 C 0.2004(2) 0.45519(12) 0.2398(2) 0.0276(6) Uani 1 d . . .
H2A H 0.2162 0.4342 0.1930 0.033 Uiso 1 calc . . R
H2B H 0.1350 0.4622 0.2272 0.033 Uiso 1 calc . . R
C3 C 0.2284(2) 0.43014(13) 0.3273(2) 0.0327(7) Uani 1 d . . .
H3A H 0.1788 0.4303 0.3602 0.039 Uiso 1 calc . . R
H3B H 0.2481 0.3951 0.3212 0.039 Uiso 1 calc . . R
C4 C 0.2454(2) 0.53903(11) 0.18403(18) 0.0222(5) Uani 1 d . . .
C5 C 0.3074(2) 0.53846(12) 0.12783(19) 0.0239(6) Uani 1 d . . .
C6 C 0.2978(2) 0.57360(13) 0.0622(2) 0.0281(6) Uani 1 d . . .
H6 H 0.3397 0.5738 0.0243 0.034 Uiso 1 calc . . R
C7 C 0.2284(2) 0.60854(13) 0.0502(2) 0.0306(7) Uani 1 d . . .
C8 C 0.1665(2) 0.60720(12) 0.1045(2) 0.0297(7) Uani 1 d . . .
H8 H 0.1181 0.6304 0.0956 0.036 Uiso 1 calc . . R
C9 C 0.1732(2) 0.57252(12) 0.17209(19) 0.0252(6) Uani 1 d . . .
C10 C 0.3820(2) 0.50042(12) 0.1381(2) 0.0296(6) Uani 1 d . . .
H10A H 0.4235 0.5062 0.1928 0.044 Uiso 1 calc . . GR
H10B H 0.4145 0.5036 0.0902 0.044 Uiso 1 calc . . GR
H10C H 0.3567 0.4666 0.1381 0.044 Uiso 1 calc . . GR
C11 C 0.2204(3) 0.64676(16) -0.0219(3) 0.0470(10) Uani 1 d . . .
H11A H 0.2714 0.6699 -0.0102 0.071 Uiso 1 calc . . GR
H11B H 0.1642 0.6656 -0.0253 0.071 Uiso 1 calc . . GR
H11C H 0.2202 0.6295 -0.0767 0.071 Uiso 1 calc . . GR
C12 C 0.1027(2) 0.57150(15) 0.2279(2) 0.0342(7) Uani 1 d . . .
H12A H 0.1293 0.5588 0.2853 0.051 Uiso 1 calc . . GR
H12B H 0.0532 0.5495 0.2017 0.051 Uiso 1 calc . . GR
H12C H 0.0797 0.6055 0.2331 0.051 Uiso 1 calc . . GR
C13 C 0.3574(2) 0.44838(11) 0.45254(19) 0.0222(5) Uani 1 d . . .
H13A H 0.4042 0.4743 0.4700 0.027 Uiso 1 calc . . R
H13B H 0.3882 0.4161 0.4468 0.027 Uiso 1 calc . . R
C14 C 0.3013(2) 0.44334(11) 0.52285(19) 0.0224(6) Uani 1 d . . .
H14A H 0.2557 0.4167 0.5064 0.027 Uiso 1 calc . . R
H14B H 0.2692 0.4753 0.5277 0.027 Uiso 1 calc . . R
C15 C 0.35888(19) 0.43049(11) 0.61023(18) 0.0210(5) Uani 1 d . . .
H15A H 0.4015 0.4583 0.6285 0.025 Uiso 1 calc . . R
H15B H 0.3195 0.4274 0.6535 0.025 Uiso 1 calc . . R
C16 C 0.49783(19) 0.38022(10) 0.61711(18) 0.0197(5) Uani 1 d . . .
C17 C 0.3633(2) 0.33511(11) 0.5886(2) 0.0235(6) Uani 1 d . . .
H17A H 0.3272 0.3348 0.5294 0.028 Uiso 1 calc . . R
H17B H 0.3238 0.3272 0.6303 0.028 Uiso 1 calc . . R
C18 C 0.4422(2) 0.29837(11) 0.5973(2) 0.0231(6) Uani 1 d . . .
H18A H 0.4447 0.2763 0.6482 0.028 Uiso 1 calc . . R
H18B H 0.4383 0.2774 0.5449 0.028 Uiso 1 calc . . R
C19 C 0.6122(2) 0.31531(11) 0.6220(2) 0.0225(6) Uani 1 d . . .
C20 C 0.6627(2) 0.31470(11) 0.7059(2) 0.0249(6) Uani 1 d . . .
C21 C 0.7531(2) 0.30152(12) 0.7177(2) 0.0283(6) Uani 1 d . . .
H21 H 0.7884 0.3022 0.7742 0.034 Uiso 1 calc . . R
C22 C 0.7929(2) 0.28739(12) 0.6485(2) 0.0298(7) Uani 1 d . . .
C23 C 0.7398(2) 0.28595(12) 0.5667(2) 0.0294(7) Uani 1 d . . .
H23 H 0.7659 0.2752 0.5195 0.035 Uiso 1 calc . . R
C24 C 0.6493(2) 0.29976(11) 0.5516(2) 0.0244(6) Uani 1 d . . .
C25 C 0.6206(2) 0.32803(13) 0.7826(2) 0.0313(7) Uani 1 d . . .
H25A H 0.6597 0.3166 0.8357 0.047 Uiso 1 calc . . GR
H25B H 0.5618 0.3116 0.7769 0.047 Uiso 1 calc . . GR
H25C H 0.6129 0.3645 0.7849 0.047 Uiso 1 calc . . GR
C26 C 0.8915(2) 0.27438(15) 0.6619(3) 0.0405(8) Uani 1 d . . .
H26A H 0.9269 0.3018 0.6927 0.061 Uiso 1 calc . . GR
H26B H 0.9090 0.2694 0.6058 0.061 Uiso 1 calc . . GR
H26C H 0.9026 0.2435 0.6959 0.061 Uiso 1 calc . . GR
C27 C 0.5950(2) 0.29727(14) 0.4615(2) 0.0319(7) Uani 1 d . . .
H27A H 0.6352 0.2995 0.4197 0.048 Uiso 1 calc . . GR
H27B H 0.5522 0.3253 0.4525 0.048 Uiso 1 calc . . GR
H27C H 0.5620 0.2654 0.4536 0.048 Uiso 1 calc . . GR
Ag2 Ag 0.355000(14) -0.027920(8) 0.352988(13) 0.02015(6) Uani 1 d . . .
N5 N 0.19903(18) 0.04446(9) 0.32927(18) 0.0250(5) Uani 1 d . . .
N6 N 0.32284(17) 0.08730(9) 0.34295(16) 0.0229(5) Uani 1 d . . .
N7 N 0.52566(18) 0.12082(9) 0.58046(16) 0.0232(5) Uani 1 d . . .
N8 N 0.61148(18) 0.13222(9) 0.70567(16) 0.0224(5) Uani 1 d . . .
C28 C 0.2881(2) 0.04120(11) 0.34114(18) 0.0209(5) Uani 1 d . . .
C29 C 0.1659(2) 0.09696(11) 0.3238(2) 0.0281(6) Uani 1 d . . .
H29A H 0.1370 0.1055 0.3733 0.034 Uiso 1 calc . . R
H29B H 0.1228 0.1030 0.2694 0.034 Uiso 1 calc . . R
C30 C 0.2531(2) 0.12656(11) 0.3265(2) 0.0283(6) Uani 1 d . . .
H30A H 0.2534 0.1437 0.2710 0.034 Uiso 1 calc . . R
H30B H 0.2616 0.1518 0.3735 0.034 Uiso 1 calc . . R
C31 C 0.1393(2) 0.00199(11) 0.3229(2) 0.0254(6) Uani 1 d . . .
C32 C 0.1064(2) -0.01312(12) 0.3960(2) 0.0278(6) Uani 1 d . . .
C33 C 0.0519(2) -0.05557(13) 0.3885(2) 0.0329(7) Uani 1 d . . .
H33 H 0.0304 -0.0670 0.4379 0.039 Uiso 1 calc . . R
C34 C 0.0278(2) -0.08179(12) 0.3116(3) 0.0330(7) Uani 1 d . . .
C35 C 0.0585(2) -0.06413(12) 0.2393(3) 0.0338(7) Uani 1 d . . .
H35 H 0.0409 -0.0810 0.1858 0.041 Uiso 1 calc . . R
C36 C 0.1146(2) -0.02232(12) 0.2435(2) 0.0301(7) Uani 1 d . . .
C37 C 0.1284(3) 0.01575(14) 0.4794(2) 0.0368(8) Uani 1 d . . .
H37A H 0.0910 0.0460 0.4755 0.055 Uiso 1 calc . . GR
H37B H 0.1920 0.0254 0.4901 0.055 Uiso 1 calc . . GR
H37C H 0.1165 -0.0053 0.5269 0.055 Uiso 1 calc . . GR
C38 C -0.0279(3) -0.12901(14) 0.3074(3) 0.0456(10) Uani 1 d . . .
H38A H -0.0708 -0.1259 0.3465 0.068 Uiso 1 calc . . GR
H38B H 0.0116 -0.1578 0.3246 0.068 Uiso 1 calc . . GR
H38C H -0.0607 -0.1339 0.2482 0.068 Uiso 1 calc . . GR
C39 C 0.1477(3) -0.00447(15) 0.1643(2) 0.0420(9) Uani 1 d . . .
H39A H 0.1432 0.0322 0.1607 0.063 Uiso 1 calc . . GR
H39B H 0.1108 -0.0194 0.1128 0.063 Uiso 1 calc . . GR
H39C H 0.2105 -0.0146 0.1680 0.063 Uiso 1 calc . . GR
C40 C 0.4173(2) 0.09886(12) 0.34374(19) 0.0248(6) Uani 1 d . . .
H40A H 0.4213 0.1192 0.2921 0.030 Uiso 1 calc . . R
H40B H 0.4499 0.0670 0.3394 0.030 Uiso 1 calc . . R
C41 C 0.4641(2) 0.12711(11) 0.42349(19) 0.0242(6) Uani 1 d . . .
H41A H 0.5252 0.1368 0.4157 0.029 Uiso 1 calc . . R
H41B H 0.4303 0.1582 0.4298 0.029 Uiso 1 calc . . R
C42 C 0.4714(2) 0.09601(11) 0.50546(18) 0.0229(6) Uani 1 d . . .
H42A H 0.4104 0.0898 0.5171 0.027 Uiso 1 calc . . R
H42B H 0.4987 0.0631 0.4966 0.027 Uiso 1 calc . . R
C43 C 0.58551(19) 0.09934(10) 0.64141(18) 0.0194(5) Uani 1 d . . .
C44 C 0.5030(2) 0.17264(11) 0.6028(2) 0.0282(6) Uani 1 d . . .
H44A H 0.4386 0.1756 0.6064 0.034 Uiso 1 calc . . R
H44B H 0.5171 0.1971 0.5600 0.034 Uiso 1 calc . . R
C45 C 0.5633(3) 0.18056(12) 0.6912(2) 0.0314(7) Uani 1 d . . .
H45A H 0.6055 0.2088 0.6899 0.038 Uiso 1 calc . . R
H45B H 0.5272 0.1870 0.7363 0.038 Uiso 1 calc . . R
C46 C 0.6612(2) 0.11901(11) 0.78949(18) 0.0217(5) Uani 1 d . . .
C47 C 0.7483(2) 0.13715(11) 0.81661(19) 0.0246(6) Uani 1 d . . .
C48 C 0.7926(2) 0.12611(12) 0.9004(2) 0.0272(6) Uani 1 d . . .
H48 H 0.8518 0.1386 0.9196 0.033 Uiso 1 calc . . R
C49 C 0.7527(2) 0.09742(12) 0.9561(2) 0.0267(6) Uani 1 d . . .
C50 C 0.6652(2) 0.08001(11) 0.92702(19) 0.0242(6) Uani 1 d . . .
H50 H 0.6373 0.0603 0.9647 0.029 Uiso 1 calc . . R
C51 C 0.6179(2) 0.09061(11) 0.84468(19) 0.0232(6) Uani 1 d . . .
C52 C 0.7952(2) 0.16820(13) 0.7587(2) 0.0328(7) Uani 1 d . . .
H52A H 0.8481 0.1844 0.7933 0.049 Uiso 1 calc . . GR
H52B H 0.7540 0.1939 0.7299 0.049 Uiso 1 calc . . GR
H52C H 0.8142 0.1465 0.7153 0.049 Uiso 1 calc . . GR
C53 C 0.8018(2) 0.08570(14) 1.0459(2) 0.0339(7) Uani 1 d . . .
H53A H 0.8132 0.0495 1.0512 0.051 Uiso 1 calc . . GR
H53B H 0.7651 0.0961 1.0878 0.051 Uiso 1 calc . . GR
H53C H 0.8591 0.1038 1.0571 0.051 Uiso 1 calc . . GR
C54 C 0.5223(2) 0.07363(13) 0.8184(2) 0.0296(7) Uani 1 d . . .
H54A H 0.5065 0.0517 0.8632 0.044 Uiso 1 calc . . GR
H54B H 0.5155 0.0551 0.7639 0.044 Uiso 1 calc . . GR
H54C H 0.4825 0.1029 0.8108 0.044 Uiso 1 calc . . GR
P2 P 0.34277(6) 0.27745(3) 0.31639(6) 0.03024(18) Uani 1 d . . .
F7 F 0.43775(17) 0.24954(10) 0.32770(18) 0.0547(6) Uani 1 d . . .
F8 F 0.36531(18) 0.30589(10) 0.23379(16) 0.0531(6) Uani 1 d . . .
F9 F 0.38846(16) 0.32228(8) 0.37729(16) 0.0429(5) Uani 1 d . . .
F10 F 0.3220(2) 0.24901(10) 0.39906(15) 0.0528(6) Uani 1 d . . .
F11 F 0.29740(18) 0.23283(8) 0.25615(15) 0.0464(6) Uani 1 d . . .
F12 F 0.24874(15) 0.30563(9) 0.30267(17) 0.0480(6) Uani 1 d . . .
P1 P 0.08382(6) 0.14693(4) 0.05452(7) 0.0391(2) Uani 1 d . . .
F1 F 0.16813(15) 0.12118(9) 0.11453(15) 0.0421(5) Uani 1 d . . .
F2 F 0.0736(2) 0.09847(13) -0.0065(2) 0.0726(9) Uani 1 d . . .
F3 F 0.15076(16) 0.17101(12) -0.00238(18) 0.0589(7) Uani 1 d . . .
F4 F 0.09627(19) 0.19463(10) 0.1163(2) 0.0658(8) Uani 1 d . . .
F5 F 0.01909(17) 0.12265(11) 0.1120(2) 0.0610(7) Uani 1 d . . .
F6 F 0.00020(19) 0.17308(14) -0.0046(3) 0.0808(10) Uani 1 d . . .
N9 N 0.2603(3) 0.37782(14) 0.0575(3) 0.0510(9) Uani 1 d . . .
C55 C 0.2333(3) 0.33894(15) 0.0638(3) 0.0405(8) Uani 1 d . . .
C56 C 0.1987(4) 0.28827(17) 0.0721(3) 0.0612(14) Uani 1 d . . .
H56A H 0.1329 0.2888 0.0580 0.092 Uiso 1 calc . . GR
H56B H 0.2182 0.2764 0.1314 0.092 Uiso 1 calc . . GR
H56C H 0.2218 0.2657 0.0323 0.092 Uiso 1 calc . . GR
N10 N 0.0223(4) 0.1782(2) 0.4151(4) 0.0947(19) Uani 1 d . . .
C57 C 0.0457(4) 0.2119(2) 0.3792(4) 0.0663(14) Uani 1 d . . .
C58 C 0.0820(4) 0.2516(3) 0.3370(4) 0.0776(18) Uani 1 d . . .
H58A H 0.1394 0.2622 0.3719 0.116 Uiso 1 calc . . GR
H58B H 0.0400 0.2799 0.3292 0.116 Uiso 1 calc . . GR
H58C H 0.0918 0.2401 0.2804 0.116 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
Ag1 C1 2.105(3) . ?
Ag1 C16 2.106(3) 3_666 ?
N1 C1 1.333(4) . ?
N1 C2 1.481(4) . ?
N1 C4 1.430(4) . ?
N2 C1 1.322(4) . ?
N2 C3 1.477(4) . ?
N2 C13 1.453(4) . ?
N3 C15 1.459(4) . ?
N3 C16 1.323(4) . ?
N3 C17 1.484(4) . ?
N4 C16 1.332(4) . ?
N4 C18 1.483(4) . ?
N4 C19 1.434(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.521(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.406(4) . ?
C4 C9 1.396(4) . ?
C5 C6 1.383(4) . ?
C5 C10 1.504(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(5) . ?
C7 C8 1.384(5) . ?
C7 C11 1.514(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.400(4) . ?
C9 C12 1.507(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.524(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.526(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 Ag1 2.106(3) 3_666 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.530(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.400(4) . ?
C19 C24 1.398(4) . ?
C20 C21 1.390(4) . ?
C20 C25 1.512(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.393(5) . ?
C22 C23 1.388(5) . ?
C22 C26 1.509(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.395(4) . ?
C24 C27 1.505(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
Ag2 C28 2.093(3) . ?
Ag2 C43 2.100(3) 3_656 ?
N5 C28 1.329(4) . ?
N5 C29 1.483(4) . ?
N5 C31 1.440(4) . ?
N6 C28 1.334(4) . ?
N6 C30 1.475(4) . ?
N6 C40 1.461(4) . ?
N7 C42 1.465(4) . ?
N7 C43 1.322(4) . ?
N7 C44 1.481(4) . ?
N8 C43 1.342(4) . ?
N8 C45 1.477(4) . ?
N8 C46 1.438(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.531(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.399(4) . ?
C31 C36 1.398(5) . ?
C32 C33 1.392(5) . ?
C32 C37 1.507(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.388(5) . ?
C34 C35 1.393(5) . ?
C34 C38 1.509(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.394(5) . ?
C36 C39 1.507(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.522(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.522(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 Ag2 2.100(3) 3_656 ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.532(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.394(4) . ?
C46 C51 1.406(4) . ?
C47 C48 1.397(4) . ?
C47 C52 1.505(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.387(4) . ?
C49 C50 1.397(4) . ?
C49 C53 1.503(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.390(4) . ?
C51 C54 1.498(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
P2 F7 1.599(3) . ?
P2 F8 1.598(2) . ?
P2 F9 1.606(2) . ?
P2 F10 1.590(2) . ?
P2 F11 1.595(2) . ?
P2 F12 1.588(2) . ?
P1 F1 1.595(2) . ?
P1 F2 1.601(3) . ?
P1 F3 1.608(3) . ?
P1 F4 1.592(3) . ?
P1 F5 1.592(3) . ?
P1 F6 1.586(3) . ?
N9 C55 1.125(5) . ?
C55 C56 1.463(6) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
N10 C57 1.152(8) . ?
C57 C58 1.415(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ag1 C16 177.39(11) . 3_666 ?
C1 N1 C2 112.4(2) . . ?
C1 N1 C4 125.7(2) . . ?
C4 N1 C2 121.5(2) . . ?
C1 N2 C3 112.7(2) . . ?
C1 N2 C13 126.2(2) . . ?
C13 N2 C3 121.1(2) . . ?
C15 N3 C17 121.4(2) . . ?
C16 N3 C15 126.0(2) . . ?
C16 N3 C17 112.4(2) . . ?
C16 N4 C18 112.1(2) . . ?
C16 N4 C19 123.5(2) . . ?
C19 N4 C18 123.5(2) . . ?
N1 C1 Ag1 122.5(2) . . ?
N2 C1 Ag1 128.2(2) . . ?
N2 C1 N1 109.2(2) . . ?
N1 C2 H2A 111.4 . . ?
N1 C2 H2B 111.4 . . ?
N1 C2 C3 102.1(2) . . ?
H2A C2 H2B 109.2 . . ?
C3 C2 H2A 111.4 . . ?
C3 C2 H2B 111.4 . . ?
N2 C3 C2 102.5(2) . . ?
N2 C3 H3A 111.3 . . ?
N2 C3 H3B 111.3 . . ?
C2 C3 H3A 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C5 C4 N1 119.0(3) . . ?
C9 C4 N1 119.6(3) . . ?
C9 C4 C5 121.3(3) . . ?
C4 C5 C10 121.0(3) . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 C10 120.5(3) . . ?
C5 C6 H6 119.1 . . ?
C5 C6 C7 121.7(3) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C11 120.4(3) . . ?
C8 C7 C6 118.7(3) . . ?
C8 C7 C11 120.9(3) . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(3) . . ?
C9 C8 H8 119.1 . . ?
C4 C9 C8 117.9(3) . . ?
C4 C9 C12 122.2(3) . . ?
C8 C9 C12 119.9(3) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.0 . . ?
N2 C13 H13B 109.0 . . ?
N2 C13 C14 112.8(2) . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
C13 C14 C15 112.0(2) . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
N3 C15 C14 112.9(2) . . ?
N3 C15 H15A 109.0 . . ?
N3 C15 H15B 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N3 C16 Ag1 127.1(2) . 3_666 ?
N3 C16 N4 110.0(2) . . ?
N4 C16 Ag1 123.0(2) . 3_666 ?
N3 C17 H17A 111.3 . . ?
N3 C17 H17B 111.3 . . ?
N3 C17 C18 102.3(2) . . ?
H17A C17 H17B 109.2 . . ?
C18 C17 H17A 111.3 . . ?
C18 C17 H17B 111.3 . . ?
N4 C18 C17 102.4(2) . . ?
N4 C18 H18A 111.3 . . ?
N4 C18 H18B 111.3 . . ?
C17 C18 H18A 111.3 . . ?
C17 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
C20 C19 N4 119.3(3) . . ?
C24 C19 N4 119.5(3) . . ?
C24 C19 C20 121.2(3) . . ?
C19 C20 C25 121.0(3) . . ?
C21 C20 C19 118.7(3) . . ?
C21 C20 C25 120.3(3) . . ?
C20 C21 H21 119.3 . . ?
C20 C21 C22 121.5(3) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C26 121.0(3) . . ?
C23 C22 C21 118.4(3) . . ?
C23 C22 C26 120.6(3) . . ?
C22 C23 H23 119.0 . . ?
C22 C23 C24 122.0(3) . . ?
C24 C23 H23 119.0 . . ?
C19 C24 C27 122.2(3) . . ?
C23 C24 C19 118.1(3) . . ?
C23 C24 C27 119.7(3) . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 Ag2 C43 175.96(11) . 3_656 ?
C28 N5 C29 113.1(3) . . ?
C28 N5 C31 124.4(3) . . ?
C31 N5 C29 122.4(3) . . ?
C28 N6 C30 112.5(3) . . ?
C28 N6 C40 125.1(3) . . ?
C40 N6 C30 121.3(3) . . ?
C42 N7 C44 119.5(2) . . ?
C43 N7 C42 126.6(2) . . ?
C43 N7 C44 112.8(2) . . ?
C43 N8 C45 112.7(2) . . ?
C43 N8 C46 124.3(2) . . ?
C46 N8 C45 120.9(2) . . ?
N5 C28 Ag2 122.1(2) . . ?
N5 C28 N6 109.2(3) . . ?
N6 C28 Ag2 128.7(2) . . ?
N5 C29 H29A 111.4 . . ?
N5 C29 H29B 111.4 . . ?
N5 C29 C30 101.8(2) . . ?
H29A C29 H29B 109.3 . . ?
C30 C29 H29A 111.4 . . ?
C30 C29 H29B 111.4 . . ?
N6 C30 C29 103.0(2) . . ?
N6 C30 H30A 111.2 . . ?
N6 C30 H30B 111.2 . . ?
C29 C30 H30A 111.2 . . ?
C29 C30 H30B 111.2 . . ?
H30A C30 H30B 109.1 . . ?
C32 C31 N5 119.0(3) . . ?
C36 C31 N5 119.1(3) . . ?
C36 C31 C32 121.9(3) . . ?
C31 C32 C37 121.3(3) . . ?
C33 C32 C31 117.5(3) . . ?
C33 C32 C37 121.3(3) . . ?
C32 C33 H33 118.7 . . ?
C34 C33 C32 122.6(3) . . ?
C34 C33 H33 118.7 . . ?
C33 C34 C35 118.2(3) . . ?
C33 C34 C38 120.8(4) . . ?
C35 C34 C38 121.0(4) . . ?
C34 C35 H35 119.2 . . ?
C34 C35 C36 121.7(3) . . ?
C36 C35 H35 119.2 . . ?
C31 C36 C39 121.4(3) . . ?
C35 C36 C31 118.1(3) . . ?
C35 C36 C39 120.5(3) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C40 H40A 108.6 . . ?
N6 C40 H40B 108.6 . . ?
N6 C40 C41 114.5(2) . . ?
H40A C40 H40B 107.6 . . ?
C41 C40 H40A 108.6 . . ?
C41 C40 H40B 108.6 . . ?
C40 C41 H41A 109.1 . . ?
C40 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
C42 C41 C40 112.4(2) . . ?
C42 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
N7 C42 C41 112.4(2) . . ?
N7 C42 H42A 109.1 . . ?
N7 C42 H42B 109.1 . . ?
C41 C42 H42A 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.9 . . ?
N7 C43 Ag2 130.8(2) . 3_656 ?
N7 C43 N8 109.3(2) . . ?
N8 C43 Ag2 119.8(2) . 3_656 ?
N7 C44 H44A 111.2 . . ?
N7 C44 H44B 111.2 . . ?
N7 C44 C45 102.7(2) . . ?
H44A C44 H44B 109.1 . . ?
C45 C44 H44A 111.2 . . ?
C45 C44 H44B 111.2 . . ?
N8 C45 C44 102.3(2) . . ?
N8 C45 H45A 111.3 . . ?
N8 C45 H45B 111.3 . . ?
C44 C45 H45A 111.3 . . ?
C44 C45 H45B 111.3 . . ?
H45A C45 H45B 109.2 . . ?
C47 C46 N8 120.0(3) . . ?
C47 C46 C51 121.4(3) . . ?
C51 C46 N8 118.5(3) . . ?
C46 C47 C48 118.5(3) . . ?
C46 C47 C52 122.1(3) . . ?
C48 C47 C52 119.4(3) . . ?
C47 C48 H48 119.1 . . ?
C49 C48 C47 121.8(3) . . ?
C49 C48 H48 119.1 . . ?
C48 C49 C50 118.3(3) . . ?
C48 C49 C53 120.9(3) . . ?
C50 C49 C53 120.8(3) . . ?
C49 C50 H50 119.0 . . ?
C51 C50 C49 122.1(3) . . ?
C51 C50 H50 119.0 . . ?
C46 C51 C54 122.0(3) . . ?
C50 C51 C46 118.0(3) . . ?
C50 C51 C54 120.0(3) . . ?
C47 C52 H52A 109.5 . . ?
C47 C52 H52B 109.5 . . ?
C47 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C49 C53 H53A 109.5 . . ?
C49 C53 H53B 109.5 . . ?
C49 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
F7 P2 F9 90.08(14) . . ?
F8 P2 F7 89.23(16) . . ?
F8 P2 F9 90.08(14) . . ?
F10 P2 F7 89.95(16) . . ?
F10 P2 F8 179.12(17) . . ?
F10 P2 F9 89.60(13) . . ?
F10 P2 F11 90.24(13) . . ?
F11 P2 F7 89.88(14) . . ?
F11 P2 F8 90.09(14) . . ?
F11 P2 F9 179.83(15) . . ?
F12 P2 F7 178.48(16) . . ?
F12 P2 F8 89.29(15) . . ?
F12 P2 F9 90.28(13) . . ?
F12 P2 F10 91.53(15) . . ?
F12 P2 F11 89.77(14) . . ?
F1 P1 F2 89.26(16) . . ?
F1 P1 F3 89.13(13) . . ?
F2 P1 F3 89.21(18) . . ?
F4 P1 F1 89.42(16) . . ?
F4 P1 F2 178.65(19) . . ?
F4 P1 F3 90.50(17) . . ?
F4 P1 F5 89.43(17) . . ?
F5 P1 F1 89.81(14) . . ?
F5 P1 F2 90.84(18) . . ?
F5 P1 F3 178.94(16) . . ?
F6 P1 F1 179.4(2) . . ?
F6 P1 F2 91.4(2) . . ?
F6 P1 F3 90.79(17) . . ?
F6 P1 F4 90.0(2) . . ?
F6 P1 F5 90.26(17) . . ?
N9 C55 C56 179.7(5) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N10 C57 C58 175.0(7) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?

_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_75cv55b
_database_code_depnum_ccdc_archive 'CCDC 1493767'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-03-24
_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         'C50 H64 Ag2 N8, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C54 H70 Ag2 F12 N10 P2'
_chemical_formula_weight         1364.88
_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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   13.015(2)
_cell_length_b                   13.237(1)
_cell_length_c                   19.112(2)
_cell_angle_alpha                74.10(1)
_cell_angle_beta                 83.16(1)
_cell_angle_gamma                68.73(1)
_cell_volume                     2950.3(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21242
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      1.79
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 Low data completion ration is due to the limitations of the instrument available ad the Australian Synchrotron operating under rotation data collection with a fixed detector and affects some high angle data. 
;
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32622
_diffrn_reflns_theta_full        29.90
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         1.79
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                11943
_reflns_number_total             15189
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.669
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1131P)²+5.2465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2104
_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:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
 C27(H27A,H27B), C28(H28A,H28B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C21(H21), C31(H31), C33(H33), C44(H44), C46(H46)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_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
Ag1 Ag 0.35250(2) 1.00533(2) 0.203254(16) 0.02785(10) Uani 1 d . . .
Ag2 Ag 0.60641(2) 0.85690(3) 0.188304(16) 0.02916(11) Uani 1 d . . .
N1 N 0.2597(3) 1.2585(3) 0.17998(19) 0.0317(7) Uani 1 d . . .
N2 N 0.4177(3) 1.2107(3) 0.12450(19) 0.0321(7) Uani 1 d . . .
N3 N 0.6020(3) 1.0991(3) 0.16306(19) 0.0310(7) Uani 1 d . . .
N4 N 0.6751(3) 0.9948(3) 0.2664(2) 0.0338(8) Uani 1 d . . .
N5 N 0.2741(3) 0.8177(4) 0.2898(2) 0.0354(8) Uani 1 d . . .
N6 N 0.3437(3) 0.7829(3) 0.1871(2) 0.0314(7) Uani 1 d . . .
N7 N 0.5231(3) 0.6980(3) 0.13654(19) 0.0317(7) Uani 1 d . . .
N8 N 0.6926(3) 0.6183(3) 0.1708(2) 0.0326(7) Uani 1 d . . .
C1 C 0.3447(3) 1.1715(3) 0.1676(2) 0.0276(7) Uani 1 d . . .
C2 C 0.2785(4) 1.3665(4) 0.1496(3) 0.0379(10) Uani 1 d . . .
H2A H 0.2943 1.3949 0.1884 0.046 Uiso 1 calc . . R
H2B H 0.2142 1.4238 0.1220 0.046 Uiso 1 calc . . R
C3 C 0.3790(4) 1.3341(4) 0.0996(3) 0.0412(11) Uani 1 d . . .
H3A H 0.3583 1.3603 0.0478 0.049 Uiso 1 calc . . R
H3B H 0.4354 1.3641 0.1066 0.049 Uiso 1 calc . . R
C4 C 0.1642(3) 1.2547(3) 0.2250(2) 0.0289(8) Uani 1 d . . .
C5 C 0.1698(3) 1.2298(3) 0.3009(2) 0.0293(8) Uani 1 d . . .
C6 C 0.0728(4) 1.2373(4) 0.3412(3) 0.0362(9) Uani 1 d . . .
H6 H 0.0748 1.2216 0.3927 0.043 Uiso 1 calc . . R
C7 C -0.0275(4) 1.2671(4) 0.3085(3) 0.0392(10) Uani 1 d . . .
C8 C -0.0298(4) 1.2889(4) 0.2336(3) 0.0405(10) Uani 1 d . . .
H8 H -0.0977 1.3075 0.2110 0.049 Uiso 1 calc . . R
C9 C 0.0648(4) 1.2842(4) 0.1906(2) 0.0334(9) Uani 1 d . . .
C10 C 0.2768(4) 1.1936(4) 0.3382(3) 0.0402(10) Uani 1 d . . .
H10A H 0.3198 1.2402 0.3118 0.060 Uiso 1 calc . . GR
H10B H 0.3185 1.1150 0.3390 0.060 Uiso 1 calc . . GR
H10C H 0.2620 1.2020 0.3881 0.060 Uiso 1 calc . . GR
C11 C -0.1316(5) 1.2742(5) 0.3549(4) 0.0587(16) Uani 1 d . . .
H11A H -0.1135 1.2171 0.4011 0.088 Uiso 1 calc . . GR
H11B H -0.1847 1.2614 0.3292 0.088 Uiso 1 calc . . GR
H11C H -0.1638 1.3485 0.3646 0.088 Uiso 1 calc . . GR
C12 C 0.0606(5) 1.3098(5) 0.1091(3) 0.0482(12) Uani 1 d . . .
H12A H 0.0673 1.3835 0.0875 0.072 Uiso 1 calc . . GR
H12B H -0.0098 1.3102 0.0954 0.072 Uiso 1 calc . . GR
H12C H 0.1214 1.2526 0.0912 0.072 Uiso 1 calc . . GR
C13 C 0.5259(3) 1.1400(4) 0.1038(2) 0.0332(8) Uani 1 d . . .
H13A H 0.5187 1.0758 0.0904 0.040 Uiso 1 calc . . R
H13B H 0.5553 1.1836 0.0608 0.040 Uiso 1 calc . . R
C14 C 0.6256(3) 0.9970(4) 0.2088(2) 0.0295(8) Uani 1 d . . .
C15 C 0.6222(4) 1.1786(4) 0.1956(3) 0.0374(9) Uani 1 d . . .
H15A H 0.5524 1.2298 0.2116 0.045 Uiso 1 calc . . R
H15B H 0.6621 1.2231 0.1611 0.045 Uiso 1 calc . . R
C16 C 0.6927(4) 1.1012(4) 0.2599(3) 0.0390(10) Uani 1 d . . .
H16A H 0.7713 1.0931 0.2500 0.047 Uiso 1 calc . . R
H16B H 0.6674 1.1283 0.3045 0.047 Uiso 1 calc . . R
C17 C 0.7181(4) 0.8999(4) 0.3267(2) 0.0330(9) Uani 1 d . . .
C18 C 0.8260(4) 0.8271(4) 0.3218(2) 0.0335(9) Uani 1 d . . .
C19 C 0.8681(4) 0.7416(4) 0.3839(3) 0.0369(10) Uani 1 d . . .
H19 H 0.9423 0.6927 0.3828 0.044 Uiso 1 calc . . R
C20 C 0.8047(4) 0.7259(4) 0.4474(3) 0.0375(10) Uani 1 d . . .
C21 C 0.6970(4) 0.7975(4) 0.4487(2) 0.0362(9) Uani 1 d . . .
H21 H 0.6518 0.7853 0.4908 0.043 Uiso 1 calc . . R
C22 C 0.6529(4) 0.8879(4) 0.3891(2) 0.0337(9) Uani 1 d . . .
C23 C 0.8928(4) 0.8366(4) 0.2518(3) 0.0388(10) Uani 1 d . . .
H23A H 0.8866 0.9149 0.2310 0.058 Uiso 1 calc . . GR
H23B H 0.8649 0.8104 0.2173 0.058 Uiso 1 calc . . GR
H23C H 0.9703 0.7906 0.2615 0.058 Uiso 1 calc . . GR
C24 C 0.8521(5) 0.6303(5) 0.5124(3) 0.0468(12) Uani 1 d . . .
H24A H 0.9136 0.6406 0.5310 0.070 Uiso 1 calc . . GR
H24B H 0.8785 0.5595 0.4979 0.070 Uiso 1 calc . . GR
H24C H 0.7948 0.6288 0.5506 0.070 Uiso 1 calc . . GR
C25 C 0.5376(4) 0.9704(4) 0.3935(3) 0.0425(10) Uani 1 d . . .
H25A H 0.5037 0.9474 0.4409 0.064 Uiso 1 calc . . GR
H25B H 0.4934 0.9722 0.3548 0.064 Uiso 1 calc . . GR
H25C H 0.5409 1.0451 0.3875 0.064 Uiso 1 calc . . GR
C26 C 0.3284(3) 0.8518(3) 0.2304(2) 0.0292(8) Uani 1 d . . .
C27 C 0.2502(4) 0.7159(4) 0.2908(3) 0.0376(9) Uani 1 d . . .
H27A H 0.1703 0.7286 0.2976 0.045 Uiso 1 calc . . R
H27B H 0.2909 0.6512 0.3295 0.045 Uiso 1 calc . . R
C28 C 0.2913(5) 0.6986(5) 0.2153(3) 0.0462(12) Uani 1 d . . .
H28A H 0.3450 0.6221 0.2184 0.055 Uiso 1 calc . . R
H28B H 0.2294 0.7115 0.1846 0.055 Uiso 1 calc . . R
C29 C 0.2518(4) 0.8620(4) 0.3531(2) 0.0326(8) Uani 1 d . . .
C30 C 0.3355(4) 0.8276(4) 0.4023(3) 0.0413(11) Uani 1 d . . .
C31 C 0.3112(4) 0.8682(4) 0.4648(3) 0.0404(10) Uani 1 d . . .
H31 H 0.3669 0.8440 0.4996 0.049 Uiso 1 calc . . R
C32 C 0.2082(4) 0.9427(4) 0.4774(2) 0.0341(9) Uani 1 d . . .
C33 C 0.1268(4) 0.9741(4) 0.4272(2) 0.0314(8) Uani 1 d . . .
H33 H 0.0554 1.0238 0.4357 0.038 Uiso 1 calc . . R
C34 C 0.1467(3) 0.9348(4) 0.3646(2) 0.0298(8) Uani 1 d . . .
C35 C 0.4507(4) 0.7521(6) 0.3860(4) 0.0602(17) Uani 1 d . . .
H35A H 0.4885 0.7967 0.3506 0.090 Uiso 1 calc . . GR
H35B H 0.4452 0.6937 0.3658 0.090 Uiso 1 calc . . GR
H35C H 0.4925 0.7173 0.4309 0.090 Uiso 1 calc . . GR
C36 C 0.1856(5) 0.9912(5) 0.5428(3) 0.0470(12) Uani 1 d . . .
H36A H 0.2215 1.0469 0.5354 0.071 Uiso 1 calc . . GR
H36B H 0.2146 0.9312 0.5863 0.071 Uiso 1 calc . . GR
H36C H 0.1058 1.0270 0.5491 0.071 Uiso 1 calc . . GR
C37 C 0.0564(4) 0.9714(5) 0.3112(3) 0.0437(11) Uani 1 d . . .
H37A H 0.0157 0.9192 0.3242 0.065 Uiso 1 calc . . GR
H37B H 0.0886 0.9723 0.2621 0.065 Uiso 1 calc . . GR
H37C H 0.0059 1.0467 0.3125 0.065 Uiso 1 calc . . GR
C38 C 0.4146(3) 0.7827(4) 0.1226(2) 0.0301(8) Uani 1 d . . .
H38A H 0.3797 0.7694 0.0843 0.036 Uiso 1 calc . . R
H38B H 0.4224 0.8572 0.1041 0.036 Uiso 1 calc . . R
C39 C 0.6061(3) 0.7118(4) 0.1628(2) 0.0292(8) Uani 1 d . . .
C40 C 0.6694(4) 0.5275(4) 0.1527(3) 0.0384(10) Uani 1 d . . .
H40A H 0.6732 0.4652 0.1963 0.046 Uiso 1 calc . . R
H40B H 0.7216 0.4983 0.1149 0.046 Uiso 1 calc . . R
C41 C 0.5519(4) 0.5862(4) 0.1244(2) 0.0350(9) Uani 1 d . . .
H41A H 0.5497 0.5899 0.0722 0.042 Uiso 1 calc . . R
H41B H 0.5016 0.5477 0.1522 0.042 Uiso 1 calc . . R
C42 C 0.7972(3) 0.5998(4) 0.1988(2) 0.0319(8) Uani 1 d . . .
C43 C 0.8087(3) 0.5732(4) 0.2743(2) 0.0311(8) Uani 1 d . . .
C44 C 0.9136(3) 0.5462(4) 0.2999(2) 0.0315(8) Uani 1 d . . .
H44 H 0.9240 0.5250 0.3510 0.038 Uiso 1 calc . . R
C45 C 1.0032(3) 0.5493(4) 0.2534(2) 0.0325(8) Uani 1 d . . .
C46 C 0.9876(4) 0.5795(4) 0.1786(2) 0.0347(9) Uani 1 d . . .
H46 H 1.0478 0.5851 0.1463 0.042 Uiso 1 calc . . R
C47 C 0.8860(4) 0.6017(4) 0.1500(2) 0.0321(8) Uani 1 d . . .
C48 C 0.7127(4) 0.5770(5) 0.3265(3) 0.0400(10) Uani 1 d . . .
H48A H 0.6665 0.6551 0.3237 0.060 Uiso 1 calc . . GR
H48B H 0.7397 0.5404 0.3761 0.060 Uiso 1 calc . . GR
H48C H 0.6692 0.5380 0.3138 0.060 Uiso 1 calc . . GR
C49 C 1.1140(4) 0.5240(4) 0.2836(3) 0.0370(9) Uani 1 d . . .
H49A H 1.1600 0.5544 0.2454 0.055 Uiso 1 calc . . GR
H49B H 1.1501 0.4427 0.3004 0.055 Uiso 1 calc . . GR
H49C H 1.1043 0.5583 0.3244 0.055 Uiso 1 calc . . GR
C50 C 0.8727(4) 0.6302(5) 0.0691(3) 0.0410(10) Uani 1 d . . .
H50A H 0.9348 0.6514 0.0441 0.061 Uiso 1 calc . . GR
H50B H 0.8036 0.6928 0.0554 0.061 Uiso 1 calc . . GR
H50C H 0.8710 0.5650 0.0551 0.061 Uiso 1 calc . . GR
P2 P 0.48718(10) 0.38172(11) 0.33969(7) 0.0387(3) Uani 1 d . . .
F7 F 0.4857(3) 0.5087(3) 0.3137(3) 0.0781(13) Uani 1 d . . .
F8 F 0.3627(3) 0.4287(3) 0.3615(3) 0.0801(13) Uani 1 d . . .
F9 F 0.4423(5) 0.3970(4) 0.2609(2) 0.0878(14) Uani 1 d . . .
F10 F 0.6087(3) 0.3398(4) 0.3067(4) 0.104(2) Uani 1 d . . .
F11 F 0.5317(6) 0.3717(5) 0.4126(3) 0.126(3) Uani 1 d . . .
F12 F 0.4889(3) 0.2574(3) 0.3605(3) 0.0683(11) Uani 1 d . . .
P1 P 0.76815(9) 1.32421(10) 0.00362(6) 0.0335(2) Uani 1 d . . .
F1 F 0.8072(3) 1.4274(3) -0.00086(18) 0.0574(9) Uani 1 d . . .
F2 F 0.7175(3) 1.3830(3) -0.07538(17) 0.0568(9) Uani 1 d . . .
F3 F 0.8827(3) 1.2627(4) -0.0297(2) 0.0699(11) Uani 1 d . . .
F4 F 0.8153(3) 1.2678(3) 0.08379(18) 0.0620(10) Uani 1 d . . .
F5 F 0.6524(3) 1.3852(3) 0.0387(2) 0.0619(9) Uani 1 d . . .
F6 F 0.7291(3) 1.2211(3) 0.00871(17) 0.0481(7) Uani 1 d . . .
N9 N 0.1245(8) 0.6635(9) 0.4667(5) 0.112(3) Uani 1 d . . .
C51 C 0.2178(8) 0.6174(8) 0.4779(4) 0.078(2) Uani 1 d . . .
C52 C 0.3353(7) 0.5583(8) 0.4926(4) 0.082(2) Uani 1 d . . .
H52A H 0.3594 0.5933 0.5235 0.124 Uiso 1 calc . . GR
H52B H 0.3776 0.5624 0.4465 0.124 Uiso 1 calc . . GR
H52C H 0.3475 0.4798 0.5175 0.124 Uiso 1 calc . . GR
N10 N 0.6661(8) 0.9402(6) -0.0108(4) 0.098(3) Uani 1 d . . .
C53 C 0.7470(8) 0.9416(7) 0.0041(5) 0.079(2) Uani 1 d . . .
C54 C 0.8506(11) 0.9424(11) 0.0242(9) 0.143(5) Uani 1 d . . .
H54A H 0.8886 0.9722 -0.0195 0.215 Uiso 1 calc . . GR
H54B H 0.8970 0.8659 0.0474 0.215 Uiso 1 calc . . GR
H54C H 0.8362 0.9897 0.0583 0.215 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
Ag1 Ag2 3.1992(12) . ?
Ag1 C1 2.085(4) . ?
Ag1 C26 2.085(4) . ?
Ag2 C14 2.100(4) . ?
Ag2 C39 2.109(4) . ?
N1 C1 1.329(6) . ?
N1 C2 1.485(6) . ?
N1 C4 1.433(5) . ?
N2 C1 1.337(5) . ?
N2 C3 1.477(6) . ?
N2 C13 1.459(6) . ?
N3 C13 1.448(5) . ?
N3 C14 1.342(5) . ?
N3 C15 1.471(6) . ?
N4 C14 1.328(5) . ?
N4 C16 1.477(6) . ?
N4 C17 1.439(5) . ?
N5 C26 1.323(6) . ?
N5 C27 1.484(6) . ?
N5 C29 1.440(6) . ?
N6 C26 1.341(6) . ?
N6 C28 1.462(6) . ?
N6 C38 1.450(6) . ?
N7 C38 1.448(5) . ?
N7 C39 1.331(5) . ?
N7 C41 1.467(6) . ?
N8 C39 1.322(6) . ?
N8 C40 1.473(6) . ?
N8 C42 1.435(5) . ?
C2 C3 1.525(7) . ?
C4 C5 1.401(6) . ?
C4 C9 1.399(5) . ?
C5 C6 1.384(6) . ?
C5 C10 1.497(6) . ?
C6 C7 1.392(7) . ?
C7 C8 1.382(7) . ?
C7 C11 1.516(7) . ?
C8 C9 1.387(7) . ?
C9 C12 1.504(7) . ?
C15 C16 1.516(7) . ?
C17 C18 1.395(6) . ?
C17 C22 1.387(7) . ?
C18 C19 1.399(6) . ?
C18 C23 1.508(7) . ?
C19 C20 1.394(7) . ?
C20 C21 1.380(7) . ?
C20 C24 1.510(7) . ?
C21 C22 1.403(6) . ?
C22 C25 1.511(6) . ?
C27 C28 1.525(7) . ?
C29 C30 1.389(6) . ?
C29 C34 1.391(6) . ?
C30 C31 1.396(7) . ?
C30 C35 1.522(7) . ?
C31 C32 1.386(7) . ?
C32 C33 1.385(6) . ?
C32 C36 1.508(7) . ?
C33 C34 1.392(6) . ?
C34 C37 1.503(6) . ?
C40 C41 1.530(6) . ?
C42 C43 1.402(6) . ?
C42 C47 1.399(6) . ?
C43 C44 1.393(6) . ?
C43 C48 1.497(6) . ?
C44 C45 1.386(6) . ?
C45 C46 1.395(6) . ?
C45 C49 1.505(6) . ?
C46 C47 1.391(6) . ?
C47 C50 1.503(6) . ?
P2 F7 1.610(4) . ?
P2 F8 1.561(4) . ?
P2 F9 1.614(4) . ?
P2 F10 1.589(4) . ?
P2 F11 1.526(5) . ?
P2 F12 1.575(4) . ?
P1 F1 1.600(3) . ?
P1 F2 1.594(3) . ?
P1 F3 1.572(4) . ?
P1 F4 1.596(3) . ?
P1 F5 1.595(4) . ?
P1 F6 1.597(3) . ?
N9 C51 1.161(12) . ?
C51 C52 1.463(12) . ?
N10 C53 1.132(12) . ?
C53 C54 1.449(15) . ?

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 Ag1 Ag2 105.88(12) . . ?
C26 Ag1 Ag2 84.05(12) . . ?
C26 Ag1 C1 168.39(15) . . ?
C14 Ag2 Ag1 80.62(11) . . ?
C14 Ag2 C39 173.34(16) . . ?
C39 Ag2 Ag1 105.65(12) . . ?
C1 N1 C2 112.6(4) . . ?
C1 N1 C4 126.8(4) . . ?
C4 N1 C2 120.1(3) . . ?
C1 N2 C3 113.5(4) . . ?
C1 N2 C13 124.1(4) . . ?
C13 N2 C3 122.4(4) . . ?
C13 N3 C15 120.0(4) . . ?
C14 N3 C13 123.6(4) . . ?
C14 N3 C15 111.9(3) . . ?
C14 N4 C16 112.3(4) . . ?
C14 N4 C17 126.6(4) . . ?
C17 N4 C16 120.9(4) . . ?
C26 N5 C27 113.4(4) . . ?
C26 N5 C29 125.3(4) . . ?
C29 N5 C27 120.7(4) . . ?
C26 N6 C28 113.4(4) . . ?
C26 N6 C38 124.1(4) . . ?
C38 N6 C28 122.2(4) . . ?
C38 N7 C41 122.9(3) . . ?
C39 N7 C38 124.3(4) . . ?
C39 N7 C41 112.9(4) . . ?
C39 N8 C40 112.8(3) . . ?
C39 N8 C42 125.9(4) . . ?
C42 N8 C40 121.2(4) . . ?
N1 C1 Ag1 124.6(3) . . ?
N1 C1 N2 108.0(4) . . ?
N2 C1 Ag1 127.2(3) . . ?
N1 C2 C3 102.2(4) . . ?
N2 C3 C2 101.2(3) . . ?
C5 C4 N1 120.4(4) . . ?
C9 C4 N1 117.9(4) . . ?
C9 C4 C5 121.6(4) . . ?
C4 C5 C10 121.8(4) . . ?
C6 C5 C4 117.9(4) . . ?
C6 C5 C10 120.3(4) . . ?
C5 C6 C7 121.9(4) . . ?
C6 C7 C11 120.0(5) . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 C11 121.2(5) . . ?
C7 C8 C9 121.6(4) . . ?
C4 C9 C12 120.8(4) . . ?
C8 C9 C4 118.3(4) . . ?
C8 C9 C12 120.9(4) . . ?
N3 C13 N2 110.9(4) . . ?
N3 C14 Ag2 126.2(3) . . ?
N4 C14 Ag2 124.7(3) . . ?
N4 C14 N3 108.7(4) . . ?
N3 C15 C16 102.1(4) . . ?
N4 C16 C15 102.2(4) . . ?
C18 C17 N4 118.9(4) . . ?
C22 C17 N4 118.6(4) . . ?
C22 C17 C18 122.4(4) . . ?
C17 C18 C19 117.1(4) . . ?
C17 C18 C23 121.6(4) . . ?
C19 C18 C23 121.3(4) . . ?
C20 C19 C18 122.2(4) . . ?
C19 C20 C24 120.6(4) . . ?
C21 C20 C19 118.6(4) . . ?
C21 C20 C24 120.8(5) . . ?
C20 C21 C22 121.3(5) . . ?
C17 C22 C21 118.3(4) . . ?
C17 C22 C25 121.1(4) . . ?
C21 C22 C25 120.6(4) . . ?
N5 C26 Ag1 123.4(3) . . ?
N5 C26 N6 108.2(4) . . ?
N6 C26 Ag1 127.3(3) . . ?
N5 C27 C28 101.9(4) . . ?
N6 C28 C27 102.7(4) . . ?
C30 C29 N5 118.7(4) . . ?
C30 C29 C34 121.8(4) . . ?
C34 C29 N5 119.5(4) . . ?
C29 C30 C31 117.9(4) . . ?
C29 C30 C35 120.1(5) . . ?
C31 C30 C35 122.0(4) . . ?
C32 C31 C30 122.0(4) . . ?
C31 C32 C36 121.2(4) . . ?
C33 C32 C31 118.2(4) . . ?
C33 C32 C36 120.6(5) . . ?
C32 C33 C34 121.9(4) . . ?
C29 C34 C33 118.2(4) . . ?
C29 C34 C37 121.6(4) . . ?
C33 C34 C37 120.2(4) . . ?
N7 C38 N6 112.4(3) . . ?
N7 C39 Ag2 127.3(3) . . ?
N8 C39 Ag2 123.3(3) . . ?
N8 C39 N7 109.3(4) . . ?
N8 C40 C41 102.4(4) . . ?
N7 C41 C40 102.4(3) . . ?
C43 C42 N8 118.8(4) . . ?
C47 C42 N8 118.8(4) . . ?
C47 C42 C43 122.2(4) . . ?
C42 C43 C48 122.3(4) . . ?
C44 C43 C42 117.4(4) . . ?
C44 C43 C48 120.2(4) . . ?
C45 C44 C43 122.2(4) . . ?
C44 C45 C46 118.6(4) . . ?
C44 C45 C49 120.3(4) . . ?
C46 C45 C49 121.0(4) . . ?
C47 C46 C45 121.6(4) . . ?
C42 C47 C50 121.7(4) . . ?
C46 C47 C42 117.8(4) . . ?
C46 C47 C50 120.4(4) . . ?
F7 P2 F9 88.7(3) . . ?
F8 P2 F7 88.2(2) . . ?
F8 P2 F9 84.9(3) . . ?
F8 P2 F10 172.4(3) . . ?
F8 P2 F12 92.7(2) . . ?
F10 P2 F7 89.8(2) . . ?
F10 P2 F9 87.7(3) . . ?
F11 P2 F7 88.8(3) . . ?
F11 P2 F8 96.1(4) . . ?
F11 P2 F9 177.3(4) . . ?
F11 P2 F10 91.2(4) . . ?
F11 P2 F12 94.1(3) . . ?
F12 P2 F7 176.8(3) . . ?
F12 P2 F9 88.3(3) . . ?
F12 P2 F10 88.9(2) . . ?
F2 P1 F1 89.84(17) . . ?
F2 P1 F4 178.1(2) . . ?
F2 P1 F5 89.6(2) . . ?
F2 P1 F6 90.52(17) . . ?
F3 P1 F1 89.7(2) . . ?
F3 P1 F2 91.3(2) . . ?
F3 P1 F4 90.6(2) . . ?
F3 P1 F5 179.1(2) . . ?
F3 P1 F6 90.5(2) . . ?
F4 P1 F1 89.88(18) . . ?
F4 P1 F6 89.75(17) . . ?
F5 P1 F1 90.7(2) . . ?
F5 P1 F4 88.6(2) . . ?
F5 P1 F6 89.2(2) . . ?
F6 P1 F1 179.60(18) . . ?
N9 C51 C52 179.5(11) . . ?
N10 C53 C54 179.3(13) . . ?

_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_79cv93a
_database_code_depnum_ccdc_archive 'CCDC 1493766'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-03-23
_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         'C29 H38 N6 Pd, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C31 H41 F12 N7 P2 Pd'
_chemical_formula_weight         908.05
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   24.136(2)
_cell_length_b                   6.839(1)
_cell_length_c                   24.481(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.25(6)
_cell_angle_gamma                90.00
_cell_volume                     3712.8(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    30991
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      1.52
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 High residual data peaks due to absorbtion correction issues limited by the availability of resources at the Australian Synchrotron.
;
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40557
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.52
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                9911
_reflns_number_total             10748
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.760
_refine_diff_density_min         -3.142
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1173
_refine_ls_restrained_S_all      1.094
_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)+(0.1255P)²+80.4366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3132
_refine_ls_wR_factor_ref         0.3158
_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:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C21(H21)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C)
;
_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 0.23639(2) 0.79056(7) 0.49592(2) 0.01512(17) Uani 1 d . . .
N1 N 0.3024(3) 0.8687(10) 0.6265(3) 0.0194(11) Uani 1 d . . .
N2 N 0.2164(3) 0.7264(9) 0.6048(3) 0.0176(10) Uani 1 d . . .
N3 N 0.1262(3) 0.7402(9) 0.5179(3) 0.0162(10) Uani 1 d . . .
N4 N 0.1048(3) 0.8895(9) 0.4342(3) 0.0183(11) Uani 1 d . . .
N5 N 0.3256(3) 0.7584(10) 0.5096(3) 0.0213(11) Uani 1 d . . .
N6 N 0.2238(3) 0.7742(10) 0.4076(3) 0.0213(12) Uani 1 d . . .
C1 C 0.2531(3) 0.8019(10) 0.5821(3) 0.0182(12) Uani 1 d . . .
C2 C 0.2953(3) 0.8587(13) 0.6836(3) 0.0238(14) Uani 1 d . . .
H2A H 0.2863 0.9891 0.6956 0.029 Uiso 1 calc . . R
H2B H 0.3321 0.8060 0.7155 0.029 Uiso 1 calc . . R
C3 C 0.2429(3) 0.7219(11) 0.6701(3) 0.0220(13) Uani 1 d . . .
H3A H 0.2565 0.5887 0.6854 0.026 Uiso 1 calc . . R
H3B H 0.2143 0.7703 0.6868 0.026 Uiso 1 calc . . R
C4 C 0.3541(3) 0.9656(11) 0.6230(3) 0.0202(13) Uani 1 d . . .
C5 C 0.3478(3) 1.1452(13) 0.5952(4) 0.0267(15) Uani 1 d . . .
C6 C 0.3983(4) 1.2304(13) 0.5909(4) 0.0283(16) Uani 1 d . . .
H6 H 0.3942 1.3525 0.5711 0.034 Uiso 1 calc . . R
C7 C 0.4546(3) 1.1416(14) 0.6145(4) 0.0277(15) Uani 1 d . . .
C8 C 0.4601(3) 0.9638(14) 0.6433(3) 0.0263(15) Uani 1 d . . .
H8 H 0.4986 0.9034 0.6603 0.032 Uiso 1 calc . . R
C9 C 0.4104(3) 0.8706(13) 0.6479(3) 0.0245(14) Uani 1 d . . .
C10 C 0.2886(4) 1.2504(16) 0.5662(6) 0.044(3) Uani 1 d . . .
H10A H 0.2650 1.1895 0.5277 0.065 Uiso 1 calc . . GR
H10B H 0.2960 1.3879 0.5601 0.065 Uiso 1 calc . . GR
H10C H 0.2661 1.2424 0.5918 0.065 Uiso 1 calc . . GR
C11 C 0.5079(4) 1.2369(18) 0.6075(5) 0.038(2) Uani 1 d . . .
H11A H 0.5241 1.3400 0.6374 0.057 Uiso 1 calc . . GR
H11B H 0.4949 1.2939 0.5677 0.057 Uiso 1 calc . . GR
H11C H 0.5391 1.1386 0.6129 0.057 Uiso 1 calc . . GR
C12 C 0.4171(4) 0.6725(14) 0.6770(4) 0.0312(17) Uani 1 d . . .
H12A H 0.4523 0.6055 0.6753 0.047 Uiso 1 calc . . GR
H12B H 0.3808 0.5945 0.6560 0.047 Uiso 1 calc . . GR
H12C H 0.4226 0.6887 0.7186 0.047 Uiso 1 calc . . GR
C13 C 0.1599(3) 0.6275(10) 0.5707(3) 0.0179(12) Uani 1 d . . .
H13A H 0.1682 0.4953 0.5593 0.021 Uiso 1 calc . . R
H13B H 0.1359 0.6130 0.5953 0.021 Uiso 1 calc . . R
C14 C 0.1493(3) 0.8139(10) 0.4806(3) 0.0174(12) Uani 1 d . . .
C15 C 0.0606(3) 0.7495(12) 0.4937(3) 0.0210(13) Uani 1 d . . .
H15A H 0.0459 0.8044 0.5230 0.025 Uiso 1 calc . . R
H15B H 0.0424 0.6189 0.4810 0.025 Uiso 1 calc . . R
C16 C 0.0473(3) 0.8841(13) 0.4416(3) 0.0255(14) Uani 1 d . . .
H16A H 0.0145 0.8315 0.4056 0.031 Uiso 1 calc . . R
H16B H 0.0358 1.0159 0.4502 0.031 Uiso 1 calc . . R
C17 C 0.1105(3) 0.9961(11) 0.3860(3) 0.0188(12) Uani 1 d . . .
C18 C 0.0901(3) 0.9082(12) 0.3298(3) 0.0224(13) Uani 1 d . . .
C19 C 0.0997(3) 1.0094(13) 0.2846(3) 0.0244(14) Uani 1 d . . .
H19 H 0.0859 0.9539 0.2459 0.029 Uiso 1 calc . . R
C20 C 0.1289(4) 1.1882(13) 0.2949(4) 0.0265(15) Uani 1 d . . .
C21 C 0.1471(4) 1.2718(12) 0.3510(4) 0.0254(15) Uani 1 d . . .
H21 H 0.1676 1.3939 0.3583 0.030 Uiso 1 calc . . R
C22 C 0.1363(3) 1.1822(11) 0.3965(3) 0.0211(13) Uani 1 d . . .
C23 C 0.0596(4) 0.7122(12) 0.3184(4) 0.0278(16) Uani 1 d . . .
H23A H 0.0176 0.7276 0.3137 0.042 Uiso 1 calc . . GR
H23B H 0.0807 0.6250 0.3520 0.042 Uiso 1 calc . . GR
H23C H 0.0607 0.6558 0.2820 0.042 Uiso 1 calc . . GR
C24 C 0.1427(5) 1.2895(17) 0.2466(4) 0.038(2) Uani 1 d . . .
H24A H 0.1333 1.2013 0.2126 0.057 Uiso 1 calc . . GR
H24B H 0.1855 1.3245 0.2621 0.057 Uiso 1 calc . . GR
H24C H 0.1182 1.4082 0.2340 0.057 Uiso 1 calc . . GR
C25 C 0.1489(4) 1.2892(13) 0.4544(4) 0.0306(17) Uani 1 d . . .
H25A H 0.1148 1.3745 0.4499 0.046 Uiso 1 calc . . GR
H25B H 0.1855 1.3682 0.4646 0.046 Uiso 1 calc . . GR
H25C H 0.1546 1.1941 0.4861 0.046 Uiso 1 calc . . GR
C26 C 0.3717(4) 0.7532(12) 0.5072(3) 0.0233(13) Uani 1 d . . .
C27 C 0.4312(4) 0.7458(16) 0.5038(4) 0.0325(18) Uani 1 d . . .
H27A H 0.4305 0.6483 0.4742 0.049 Uiso 1 calc . . GR
H27B H 0.4619 0.7097 0.5427 0.049 Uiso 1 calc . . GR
H27C H 0.4409 0.8744 0.4922 0.049 Uiso 1 calc . . GR
C28 C 0.2301(3) 0.7767(12) 0.3643(3) 0.0225(13) Uani 1 d . . .
C29 C 0.2383(4) 0.7787(15) 0.3086(4) 0.0301(17) Uani 1 d . . .
H29A H 0.1995 0.7543 0.2756 0.045 Uiso 1 calc . . GR
H29B H 0.2670 0.6767 0.3093 0.045 Uiso 1 calc . . GR
H29C H 0.2537 0.9067 0.3032 0.045 Uiso 1 calc . . GR
P2 P 0.64002(10) 0.7341(4) 0.61267(10) 0.0280(4) Uani 1 d . . .
F7 F 0.6082(4) 0.7517(16) 0.6579(4) 0.072(2) Uani 1 d . . .
F8 F 0.5772(4) 0.7330(14) 0.5569(4) 0.070(3) Uani 1 d . . .
F9 F 0.6431(4) 0.9645(11) 0.6072(4) 0.062(2) Uani 1 d . . .
F10 F 0.7033(3) 0.7332(12) 0.6680(3) 0.0542(19) Uani 1 d . . .
F11 F 0.6371(4) 0.5013(11) 0.6186(4) 0.065(2) Uani 1 d . . .
F12 F 0.6720(5) 0.706(2) 0.5685(4) 0.083(3) Uani 1 d . . .
P1 P 0.36815(8) 0.6734(3) 0.85142(8) 0.0186(3) Uani 1 d . . .
F1 F 0.3185(2) 0.6636(10) 0.8796(2) 0.0339(11) Uani 1 d . . .
F2 F 0.3440(2) 0.8859(8) 0.8246(2) 0.0315(11) Uani 1 d . . .
F3 F 0.4150(2) 0.7699(9) 0.9111(2) 0.0290(10) Uani 1 d . . .
F4 F 0.3921(3) 0.4613(8) 0.8771(2) 0.0309(10) Uani 1 d . . .
F5 F 0.3214(2) 0.5741(8) 0.7912(2) 0.0291(10) Uani 1 d . . .
F6 F 0.4173(2) 0.6847(9) 0.8225(2) 0.0305(11) Uani 1 d . . .
N7 N 0.4964(4) 0.1354(15) 0.8940(4) 0.044(2) Uani 1 d . . .
C30 C 0.4726(4) 0.1689(13) 0.8452(5) 0.0342(18) Uani 1 d . . .
C31 C 0.4411(8) 0.218(2) 0.7830(5) 0.062(4) Uani 1 d . . .
H31A H 0.4547 0.1314 0.7588 0.093 Uiso 1 calc . . GR
H31B H 0.4498 0.3541 0.7765 0.093 Uiso 1 calc . . GR
H31C H 0.3976 0.2019 0.7715 0.093 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 N5 2.056(6) . ?
Pd1 N6 2.065(6) . ?
Pd1 C1 1.988(7) . ?
Pd1 C14 1.989(7) . ?
N1 C1 1.337(9) . ?
N1 C2 1.474(9) . ?
N1 C4 1.445(9) . ?
N2 C1 1.322(9) . ?
N2 C3 1.470(9) . ?
N2 C13 1.454(9) . ?
N3 C13 1.449(9) . ?
N3 C14 1.342(9) . ?
N3 C15 1.455(9) . ?
N4 C14 1.324(9) . ?
N4 C16 1.468(9) . ?
N4 C17 1.438(9) . ?
N5 C26 1.137(10) . ?
N6 C28 1.130(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.501(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.383(11) . ?
C4 C9 1.409(10) . ?
C5 C6 1.395(11) . ?
C5 C10 1.504(12) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(12) . ?
C7 C8 1.385(13) . ?
C7 C11 1.509(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.402(12) . ?
C9 C12 1.510(12) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.502(11) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.402(10) . ?
C17 C22 1.395(10) . ?
C18 C19 1.400(11) . ?
C18 C23 1.501(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.384(12) . ?
C20 C21 1.390(12) . ?
C20 C24 1.515(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(10) . ?
C22 C25 1.514(11) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.473(11) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.452(11) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
P2 F7 1.582(9) . ?
P2 F8 1.590(7) . ?
P2 F9 1.586(8) . ?
P2 F10 1.592(7) . ?
P2 F11 1.602(8) . ?
P2 F12 1.569(9) . ?
P1 F1 1.602(5) . ?
P1 F2 1.607(6) . ?
P1 F3 1.595(5) . ?
P1 F4 1.596(5) . ?
P1 F5 1.611(5) . ?
P1 F6 1.605(5) . ?
N7 C30 1.126(14) . ?
C30 C31 1.448(16) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Pd1 N6 82.9(2) . . ?
C1 Pd1 N5 94.1(3) . . ?
C1 Pd1 N6 176.9(3) . . ?
C1 Pd1 C14 87.3(3) . . ?
C14 Pd1 N5 177.9(3) . . ?
C14 Pd1 N6 95.7(3) . . ?
C1 N1 C2 110.8(6) . . ?
C1 N1 C4 128.5(6) . . ?
C4 N1 C2 120.2(6) . . ?
C1 N2 C3 112.8(6) . . ?
C1 N2 C13 125.0(6) . . ?
C13 N2 C3 121.5(6) . . ?
C13 N3 C15 121.6(6) . . ?
C14 N3 C13 124.6(6) . . ?
C14 N3 C15 112.7(6) . . ?
C14 N4 C16 111.8(6) . . ?
C14 N4 C17 126.4(6) . . ?
C17 N4 C16 121.0(6) . . ?
C26 N5 Pd1 167.9(6) . . ?
C28 N6 Pd1 164.6(6) . . ?
N1 C1 Pd1 128.2(5) . . ?
N2 C1 Pd1 122.8(5) . . ?
N2 C1 N1 108.8(6) . . ?
N1 C2 H2A 111.2 . . ?
N1 C2 H2B 111.2 . . ?
N1 C2 C3 102.9(6) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
N2 C3 C2 101.2(6) . . ?
N2 C3 H3A 111.5 . . ?
N2 C3 H3B 111.5 . . ?
C2 C3 H3A 111.5 . . ?
C2 C3 H3B 111.5 . . ?
H3A C3 H3B 109.4 . . ?
C5 C4 N1 120.4(6) . . ?
C5 C4 C9 121.5(7) . . ?
C9 C4 N1 118.1(7) . . ?
C4 C5 C6 118.6(7) . . ?
C4 C5 C10 123.9(7) . . ?
C6 C5 C10 117.4(8) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.8(8) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C11 120.0(9) . . ?
C8 C7 C6 118.5(7) . . ?
C8 C7 C11 121.5(8) . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(7) . . ?
C9 C8 H8 119.1 . . ?
C4 C9 C12 121.6(7) . . ?
C8 C9 C4 117.7(8) . . ?
C8 C9 C12 120.7(7) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.8 . . ?
N2 C13 H13B 109.8 . . ?
N3 C13 N2 109.5(5) . . ?
N3 C13 H13A 109.8 . . ?
N3 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
N3 C14 Pd1 122.3(5) . . ?
N4 C14 Pd1 129.3(5) . . ?
N4 C14 N3 108.3(6) . . ?
N3 C15 H15A 111.4 . . ?
N3 C15 H15B 111.4 . . ?
N3 C15 C16 101.8(6) . . ?
H15A C15 H15B 109.3 . . ?
C16 C15 H15A 111.4 . . ?
C16 C15 H15B 111.4 . . ?
N4 C16 C15 103.0(6) . . ?
N4 C16 H16A 111.2 . . ?
N4 C16 H16B 111.2 . . ?
C15 C16 H16A 111.2 . . ?
C15 C16 H16B 111.2 . . ?
H16A C16 H16B 109.1 . . ?
C18 C17 N4 118.5(7) . . ?
C22 C17 N4 119.5(6) . . ?
C22 C17 C18 122.0(7) . . ?
C17 C18 C23 121.5(7) . . ?
C19 C18 C17 117.4(7) . . ?
C19 C18 C23 121.1(7) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 C18 121.7(7) . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C21 118.8(7) . . ?
C19 C20 C24 121.0(8) . . ?
C21 C20 C24 120.1(8) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 C20 121.8(8) . . ?
C22 C21 H21 119.1 . . ?
C17 C22 C25 121.5(7) . . ?
C21 C22 C17 117.9(7) . . ?
C21 C22 C25 120.4(7) . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C27 179.6(9) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C28 C29 179.7(10) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F7 P2 F8 92.3(6) . . ?
F7 P2 F9 92.0(6) . . ?
F7 P2 F10 88.3(5) . . ?
F7 P2 F11 87.8(6) . . ?
F8 P2 F10 179.2(6) . . ?
F8 P2 F11 90.7(4) . . ?
F9 P2 F8 89.5(4) . . ?
F9 P2 F10 90.9(4) . . ?
F9 P2 F11 179.7(5) . . ?
F10 P2 F11 88.9(4) . . ?
F12 P2 F7 177.3(7) . . ?
F12 P2 F8 88.2(6) . . ?
F12 P2 F9 90.6(6) . . ?
F12 P2 F10 91.1(5) . . ?
F12 P2 F11 89.6(6) . . ?
F1 P1 F2 90.1(3) . . ?
F1 P1 F5 90.2(3) . . ?
F1 P1 F6 179.3(3) . . ?
F2 P1 F5 89.9(3) . . ?
F3 P1 F1 90.2(3) . . ?
F3 P1 F2 90.6(3) . . ?
F3 P1 F4 90.0(3) . . ?
F3 P1 F5 179.3(3) . . ?
F3 P1 F6 90.2(3) . . ?
F4 P1 F1 90.4(3) . . ?
F4 P1 F2 179.2(3) . . ?
F4 P1 F5 89.5(3) . . ?
F4 P1 F6 90.2(3) . . ?
F6 P1 F2 89.3(3) . . ?
F6 P1 F5 89.4(3) . . ?
N7 C30 C31 178.1(11) . . ?
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 . . ?

_olex2_submission_original_sample_id as79cv93a
_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_50cv44
_database_code_depnum_ccdc_archive 'CCDC 1493765'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-03-23
_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 H32 Br2 N4 Pd'
_chemical_formula_sum            'C24 H32 Br2 N4 Pd'
_chemical_formula_weight         642.76
_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'
Br Br -0.2901 2.4595 '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'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.283(6)
_cell_length_b                   14.081(1)
_cell_length_c                   12.991(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.10(1)
_cell_angle_gamma                90.00
_cell_volume                     5058.7(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    33894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      1.47
_exptl_absorpt_coefficient_mu    3.912
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50134
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         1.47
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6202
_reflns_number_total             7322
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.721
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.098
_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)+(0.0508P)²+21.7372P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1071
_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:
 C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C13(H13), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), 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
Pd1 Pd 0.140965(8) 0.001704(14) 0.100781(17) 0.01828(7) Uani 1 d . . .
Br1 Br 0.209573(12) 0.08106(2) 0.05102(2) 0.02489(8) Uani 1 d . . .
Br2 Br 0.071583(12) -0.07249(2) 0.15224(3) 0.02860(9) Uani 1 d . . .
N1 N 0.18417(9) -0.10458(17) 0.16732(19) 0.0194(5) Uani 1 d . . .
N2 N 0.24468(9) -0.20984(18) 0.19296(19) 0.0199(5) Uani 1 d . . .
N3 N 0.09957(10) 0.11093(18) 0.0372(2) 0.0236(5) Uani 1 d . . .
N4 N 0.07487(10) 0.26136(18) 0.0173(2) 0.0249(5) Uani 1 d . . .
C1 C 0.21892(11) -0.1422(2) 0.1320(2) 0.0194(5) Uani 1 d . . .
H1 H 0.2261 -0.1236 0.0667 0.023 Uiso 1 calc . . R
C2 C 0.18183(11) -0.1526(2) 0.2677(2) 0.0219(6) Uani 1 d . . .
H2A H 0.1534 -0.1953 0.2588 0.026 Uiso 1 calc . . R
H2B H 0.1800 -0.1057 0.3235 0.026 Uiso 1 calc . . R
C3 C 0.22919(12) -0.2095(2) 0.2947(2) 0.0259(6) Uani 1 d . . .
H3A H 0.2533 -0.1776 0.3502 0.031 Uiso 1 calc . . R
H3B H 0.2236 -0.2748 0.3178 0.031 Uiso 1 calc . . R
C4 C 0.29114(11) -0.2430(2) 0.1811(2) 0.0190(5) Uani 1 d . . .
C5 C 0.32990(11) -0.1796(2) 0.1911(2) 0.0200(5) Uani 1 d . . .
C6 C 0.37450(11) -0.2146(2) 0.1798(2) 0.0215(6) Uani 1 d . . .
H6 H 0.4009 -0.1720 0.1847 0.026 Uiso 1 calc . . R
C7 C 0.38152(11) -0.3109(2) 0.1614(2) 0.0207(5) Uani 1 d . . .
C8 C 0.34216(11) -0.3722(2) 0.1530(2) 0.0209(5) Uani 1 d . . .
H8 H 0.3465 -0.4379 0.1409 0.025 Uiso 1 calc . . R
C9 C 0.29667(11) -0.3398(2) 0.1620(2) 0.0191(5) Uani 1 d . . .
C10 C 0.32429(13) -0.0762(2) 0.2174(3) 0.0252(6) Uani 1 d . . .
H10A H 0.3022 -0.0453 0.1588 0.038 Uiso 1 calc . . GR
H10B H 0.3559 -0.0449 0.2291 0.038 Uiso 1 calc . . GR
H10C H 0.3112 -0.0715 0.2813 0.038 Uiso 1 calc . . GR
C11 C 0.43037(12) -0.3490(2) 0.1525(3) 0.0264(6) Uani 1 d . . .
H11A H 0.4392 -0.4020 0.2016 0.040 Uiso 1 calc . . GR
H11B H 0.4546 -0.2985 0.1697 0.040 Uiso 1 calc . . GR
H11C H 0.4290 -0.3711 0.0804 0.040 Uiso 1 calc . . GR
C12 C 0.25465(12) -0.4068(2) 0.1515(3) 0.0239(6) Uani 1 d . . .
H12A H 0.2492 -0.4224 0.2216 0.036 Uiso 1 calc . . GR
H12B H 0.2617 -0.4651 0.1163 0.036 Uiso 1 calc . . GR
H12C H 0.2256 -0.3768 0.1098 0.036 Uiso 1 calc . . GR
C13 C 0.10710(11) 0.1972(2) 0.0679(2) 0.0219(6) Uani 1 d . . .
H13 H 0.1336 0.2149 0.1225 0.026 Uiso 1 calc . . R
C14 C 0.05549(15) 0.1077(2) -0.0461(3) 0.0407(10) Uani 1 d . . .
H14A H 0.0289 0.0758 -0.0209 0.049 Uiso 1 calc . . R
H14B H 0.0614 0.0737 -0.1089 0.049 Uiso 1 calc . . R
C15 C 0.04332(15) 0.2131(3) -0.0717(3) 0.0409(10) Uani 1 d . . .
H15A H 0.0512 0.2318 -0.1396 0.049 Uiso 1 calc . . R
H15B H 0.0088 0.2267 -0.0738 0.049 Uiso 1 calc . . R
C16 C 0.08193(11) 0.3620(2) 0.0288(2) 0.0220(6) Uani 1 d . . .
C17 C 0.05087(12) 0.4134(2) 0.0788(3) 0.0249(6) Uani 1 d . . .
C18 C 0.05992(13) 0.5104(2) 0.0967(3) 0.0264(6) Uani 1 d . . .
H18 H 0.0391 0.5464 0.1303 0.032 Uiso 1 calc . . R
C19 C 0.09853(12) 0.5554(2) 0.0665(2) 0.0233(6) Uani 1 d . . .
C20 C 0.12768(12) 0.5027(2) 0.0144(3) 0.0232(6) Uani 1 d . . .
H20 H 0.1537 0.5333 -0.0081 0.028 Uiso 1 calc . . R
C21 C 0.11992(11) 0.4058(2) -0.0061(2) 0.0212(6) Uani 1 d . . .
C22 C 0.00982(13) 0.3653(3) 0.1146(3) 0.0338(8) Uani 1 d . . .
H22A H -0.0113 0.3348 0.0543 0.051 Uiso 1 calc . . GR
H22B H -0.0087 0.4124 0.1453 0.051 Uiso 1 calc . . GR
H22C H 0.0227 0.3172 0.1677 0.051 Uiso 1 calc . . GR
C23 C 0.10962(15) 0.6586(2) 0.0929(3) 0.0330(7) Uani 1 d . . .
H23A H 0.0819 0.6881 0.1148 0.049 Uiso 1 calc . . GR
H23B H 0.1160 0.6915 0.0308 0.049 Uiso 1 calc . . GR
H23C H 0.1382 0.6630 0.1504 0.049 Uiso 1 calc . . GR
C24 C 0.15287(13) 0.3512(2) -0.0629(3) 0.0291(7) Uani 1 d . . .
H24A H 0.1785 0.3933 -0.0761 0.044 Uiso 1 calc . . GR
H24B H 0.1341 0.3274 -0.1300 0.044 Uiso 1 calc . . GR
H24C H 0.1673 0.2977 -0.0192 0.044 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 Br1 2.4409(6) . ?
Pd1 Br2 2.4370(6) . ?
Pd1 N1 2.009(2) . ?
Pd1 N3 2.003(3) . ?
N1 C1 1.283(4) . ?
N1 C2 1.483(4) . ?
N2 C1 1.350(4) . ?
N2 C3 1.477(4) . ?
N2 C4 1.433(4) . ?
N3 C13 1.283(4) . ?
N3 C14 1.470(4) . ?
N4 C13 1.352(4) . ?
N4 C15 1.471(4) . ?
N4 C16 1.435(4) . ?
C2 C3 1.537(4) . ?
C4 C5 1.398(4) . ?
C4 C9 1.400(4) . ?
C5 C6 1.391(4) . ?
C5 C10 1.511(4) . ?
C6 C7 1.398(4) . ?
C7 C8 1.395(4) . ?
C7 C11 1.509(4) . ?
C8 C9 1.393(4) . ?
C9 C12 1.502(4) . ?
C14 C15 1.544(5) . ?
C16 C17 1.399(5) . ?
C16 C21 1.394(4) . ?
C17 C18 1.400(5) . ?
C17 C22 1.500(5) . ?
C18 C19 1.388(5) . ?
C19 C20 1.387(5) . ?
C19 C23 1.510(4) . ?
C20 C21 1.399(4) . ?
C21 C24 1.513(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pd1 Br1 178.114(15) . . ?
N1 Pd1 Br1 90.53(8) . . ?
N1 Pd1 Br2 90.85(8) . . ?
N3 Pd1 Br1 88.14(8) . . ?
N3 Pd1 Br2 90.44(8) . . ?
N3 Pd1 N1 177.99(10) . . ?
C1 N1 Pd1 126.6(2) . . ?
C1 N1 C2 107.7(2) . . ?
C2 N1 Pd1 125.6(2) . . ?
C1 N2 C3 107.3(2) . . ?
C1 N2 C4 124.1(3) . . ?
C4 N2 C3 123.2(2) . . ?
C13 N3 Pd1 123.7(2) . . ?
C13 N3 C14 108.5(3) . . ?
C14 N3 Pd1 127.7(2) . . ?
C13 N4 C15 108.1(3) . . ?
C13 N4 C16 123.0(3) . . ?
C16 N4 C15 125.9(3) . . ?
N1 C1 N2 116.2(3) . . ?
N1 C2 C3 103.9(2) . . ?
N2 C3 C2 101.9(2) . . ?
C5 C4 N2 120.1(3) . . ?
C5 C4 C9 121.5(3) . . ?
C9 C4 N2 118.4(3) . . ?
C4 C5 C10 121.2(3) . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 C10 120.4(3) . . ?
C5 C6 C7 121.8(3) . . ?
C6 C7 C11 121.5(3) . . ?
C8 C7 C6 118.3(3) . . ?
C8 C7 C11 120.2(3) . . ?
C9 C8 C7 121.8(3) . . ?
C4 C9 C12 120.8(3) . . ?
C8 C9 C4 118.3(3) . . ?
C8 C9 C12 120.9(3) . . ?
N3 C13 N4 115.5(3) . . ?
N3 C14 C15 104.2(3) . . ?
N4 C15 C14 101.7(3) . . ?
C17 C16 N4 118.2(3) . . ?
C21 C16 N4 120.2(3) . . ?
C21 C16 C17 121.6(3) . . ?
C16 C17 C18 118.1(3) . . ?
C16 C17 C22 120.8(3) . . ?
C18 C17 C22 121.1(3) . . ?
C19 C18 C17 121.7(3) . . ?
C18 C19 C23 120.9(3) . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 C23 120.6(3) . . ?
C19 C20 C21 122.0(3) . . ?
C16 C21 C20 118.0(3) . . ?
C16 C21 C24 122.0(3) . . ?
C20 C21 C24 120.0(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_as59cv36
_database_code_depnum_ccdc_archive 'CCDC 1493768'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-03-24
_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         'C25 H33 I3 N4 Pd, C2 H3 N'
_chemical_formula_sum            'C27 H36 I3 N5 Pd'
_chemical_formula_weight         917.71
_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'
I I -0.4742 1.8119 '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'
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                   10.721(2)
_cell_length_b                   20.800(2)
_cell_length_c                   15.020(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.83(1)
_cell_angle_gamma                90.00
_cell_volume                     3130.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17151
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      1.75
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40418
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         1.75
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3851
_reflns_number_total             5657
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.063
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0557
_refine_ls_restrained_S_all      1.021
_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)+(0.0624P)²+21.2125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1425
_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:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C14(H14), C19(H19), C21(H21)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_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
I1 I 0.34079(8) 0.40063(4) 0.33091(5) 0.0591(2) Uani 1 d . . .
I2 I 0.52824(8) 0.17696(3) 0.47401(5) 0.0537(2) Uani 1 d . . .
I3 I 0.21462(8) 0.27056(4) 0.45221(5) 0.0652(2) Uani 1 d . . .
Pd1 Pd 0.43339(8) 0.29028(4) 0.41094(5) 0.0434(2) Uani 1 d . . .
N1 N 0.5779(8) 0.2897(4) 0.2791(5) 0.0427(19) Uani 1 d . . .
N2 N 0.7131(8) 0.3211(4) 0.4180(5) 0.0423(19) Uani 1 d . . .
N3 N 0.4504(8) 0.1987(4) 0.1983(5) 0.0446(19) Uani 1 d . . .
N4 N 0.3750(8) 0.1002(4) 0.2018(6) 0.0450(19) Uani 1 d . . .
C1 C 0.5887(10) 0.3007(4) 0.3699(7) 0.044(2) Uani 1 d . . .
C2 C 0.7041(12) 0.3006(6) 0.2637(8) 0.063(3) Uani 1 d . . .
H2A H 0.6915 0.3305 0.2100 0.075 Uiso 1 calc . . R
H2B H 0.7415 0.2597 0.2506 0.075 Uiso 1 calc . . R
C3 C 0.7924(11) 0.3293(6) 0.3557(7) 0.058(3) Uani 1 d . . .
H3A H 0.8785 0.3062 0.3814 0.069 Uiso 1 calc . . R
H3B H 0.8099 0.3753 0.3478 0.069 Uiso 1 calc . . R
C4 C 0.7704(10) 0.3343(5) 0.5184(6) 0.042(2) Uani 1 d . . .
C5 C 0.8570(12) 0.2893(5) 0.5759(8) 0.060(3) Uani 1 d . . .
C6 C 0.9169(13) 0.3037(7) 0.6748(8) 0.074(4) Uani 1 d . . .
H6 H 0.9734 0.2728 0.7166 0.088 Uiso 1 calc . . R
C7 C 0.8943(12) 0.3614(6) 0.7106(7) 0.063(3) Uani 1 d . . .
C8 C 0.8125(11) 0.4072(6) 0.6494(7) 0.055(3) Uani 1 d . . .
H8 H 0.7970 0.4472 0.6743 0.067 Uiso 1 calc . . R
C9 C 0.7531(10) 0.3948(5) 0.5517(7) 0.044(2) Uani 1 d . . .
C10 C 0.8932(13) 0.2274(6) 0.5385(9) 0.069(3) Uani 1 d . . .
H10A H 0.8157 0.2115 0.4858 0.104 Uiso 1 calc . . GR
H10B H 0.9205 0.1954 0.5896 0.104 Uiso 1 calc . . GR
H10C H 0.9670 0.2353 0.5159 0.104 Uiso 1 calc . . GR
C11 C 0.9595(17) 0.3777(8) 0.8156(9) 0.097(5) Uani 1 d . . .
H11A H 0.9954 0.3384 0.8517 0.146 Uiso 1 calc . . GR
H11B H 0.8930 0.3967 0.8387 0.146 Uiso 1 calc . . GR
H11C H 1.0321 0.4084 0.8243 0.146 Uiso 1 calc . . GR
C12 C 0.6810(11) 0.4483(5) 0.4893(8) 0.053(3) Uani 1 d . . .
H12A H 0.6093 0.4309 0.4339 0.080 Uiso 1 calc . . GR
H12B H 0.7434 0.4727 0.4679 0.080 Uiso 1 calc . . GR
H12C H 0.6428 0.4768 0.5249 0.080 Uiso 1 calc . . GR
C13 C 0.4588(11) 0.2669(5) 0.2061(7) 0.049(2) Uani 1 d . . .
H13A H 0.3804 0.2831 0.2194 0.059 Uiso 1 calc . . R
H13B H 0.4547 0.2850 0.1441 0.059 Uiso 1 calc . . R
C14 C 0.3669(10) 0.1610(5) 0.2213(6) 0.046(2) Uani 1 d . . .
H14 H 0.3065 0.1768 0.2495 0.056 Uiso 1 calc . . R
C15 C 0.5382(11) 0.1576(5) 0.1647(7) 0.052(3) Uani 1 d . . .
H15A H 0.6296 0.1555 0.2127 0.062 Uiso 1 calc . . R
H15B H 0.5426 0.1739 0.1039 0.062 Uiso 1 calc . . R
C16 C 0.4708(10) 0.0923(5) 0.1512(8) 0.051(3) Uani 1 d . . .
H16A H 0.4238 0.0826 0.0828 0.061 Uiso 1 calc . . R
H16B H 0.5360 0.0577 0.1802 0.061 Uiso 1 calc . . R
C17 C 0.2946(10) 0.0506(5) 0.2206(7) 0.044(2) Uani 1 d . . .
C18 C 0.1614(10) 0.0434(5) 0.1598(8) 0.050(3) Uani 1 d . . .
C19 C 0.0865(11) -0.0040(6) 0.1846(8) 0.057(3) Uani 1 d . . .
H19 H -0.0036 -0.0107 0.1442 0.069 Uiso 1 calc . . R
C20 C 0.1373(12) -0.0406(5) 0.2636(9) 0.060(3) Uani 1 d . . .
C21 C 0.2715(12) -0.0343(5) 0.3184(8) 0.058(3) Uani 1 d . . .
H21 H 0.3082 -0.0611 0.3727 0.069 Uiso 1 calc . . R
C22 C 0.3528(10) 0.0091(5) 0.2976(7) 0.048(2) Uani 1 d . . .
C23 C 0.1040(12) 0.0848(6) 0.0734(8) 0.064(3) Uani 1 d . . .
H23A H 0.0716 0.1251 0.0912 0.097 Uiso 1 calc . . GR
H23B H 0.0298 0.0622 0.0259 0.097 Uiso 1 calc . . GR
H23C H 0.1731 0.0942 0.0467 0.097 Uiso 1 calc . . GR
C24 C 0.0503(14) -0.0901(7) 0.2874(11) 0.087(5) Uani 1 d . . .
H24A H -0.0078 -0.0686 0.3159 0.131 Uiso 1 calc . . GR
H24B H 0.1069 -0.1214 0.3326 0.131 Uiso 1 calc . . GR
H24C H -0.0046 -0.1123 0.2290 0.131 Uiso 1 calc . . GR
C25 C 0.5006(11) 0.0114(6) 0.3562(8) 0.061(3) Uani 1 d . . .
H25A H 0.5499 -0.0134 0.3239 0.092 Uiso 1 calc . . GR
H25B H 0.5163 -0.0072 0.4192 0.092 Uiso 1 calc . . GR
H25C H 0.5312 0.0561 0.3632 0.092 Uiso 1 calc . . GR
N5 N 0.8368(18) 0.0401(10) 0.467(2) 0.185(11) Uani 1 d A 1 .
C26 C 0.8313(15) -0.0157(13) 0.4683(11) 0.102(6) Uani 1 d . . .
C27 C 0.8159(17) -0.0850(8) 0.4582(11) 0.098(5) Uani 1 d A . .
H27A H 0.7743 -0.0961 0.3906 0.147 Uiso 1 calc . . GR
H27B H 0.7594 -0.1002 0.4927 0.147 Uiso 1 calc . . GR
H27C H 0.9038 -0.1056 0.4845 0.147 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
I1 Pd1 2.6173(12) . ?
I2 Pd1 2.6081(11) . ?
I3 Pd1 2.6622(12) . ?
Pd1 C1 1.982(10) . ?
N1 C1 1.348(11) . ?
N1 C2 1.469(14) . ?
N1 C13 1.435(12) . ?
N2 C1 1.340(12) . ?
N2 C3 1.481(13) . ?
N2 C4 1.439(11) . ?
N3 C13 1.424(13) . ?
N3 C14 1.324(13) . ?
N3 C15 1.486(13) . ?
N4 C14 1.308(12) . ?
N4 C16 1.488(12) . ?
N4 C17 1.435(12) . ?
C2 C3 1.494(14) . ?
C4 C5 1.385(15) . ?
C4 C9 1.390(14) . ?
C5 C6 1.424(16) . ?
C5 C10 1.508(17) . ?
C6 C7 1.373(18) . ?
C7 C8 1.395(16) . ?
C7 C11 1.519(15) . ?
C8 C9 1.400(13) . ?
C9 C12 1.483(14) . ?
C15 C16 1.518(14) . ?
C17 C18 1.403(14) . ?
C17 C22 1.400(14) . ?
C18 C19 1.404(15) . ?
C18 C23 1.495(15) . ?
C19 C20 1.350(16) . ?
C20 C21 1.386(16) . ?
C20 C24 1.516(16) . ?
C21 C22 1.366(15) . ?
C22 C25 1.515(14) . ?
N5 C26 1.16(3) . ?
C26 C27 1.45(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
I1 Pd1 I3 91.17(4) . . ?
I2 Pd1 I1 174.05(4) . . ?
I2 Pd1 I3 92.19(4) . . ?
C1 Pd1 I1 89.1(3) . . ?
C1 Pd1 I2 87.1(3) . . ?
C1 Pd1 I3 175.1(3) . . ?
C1 N1 C2 112.3(8) . . ?
C1 N1 C13 124.3(8) . . ?
C13 N1 C2 123.3(8) . . ?
C1 N2 C3 112.4(8) . . ?
C1 N2 C4 126.7(8) . . ?
C4 N2 C3 120.9(8) . . ?
C13 N3 C15 124.9(9) . . ?
C14 N3 C13 126.6(9) . . ?
C14 N3 C15 108.5(8) . . ?
C14 N4 C16 109.5(8) . . ?
C14 N4 C17 124.0(8) . . ?
C17 N4 C16 126.4(8) . . ?
N1 C1 Pd1 121.1(7) . . ?
N2 C1 Pd1 130.8(7) . . ?
N2 C1 N1 108.1(8) . . ?
N1 C2 C3 103.5(8) . . ?
N2 C3 C2 102.7(8) . . ?
C5 C4 N2 117.8(9) . . ?
C5 C4 C9 122.3(9) . . ?
C9 C4 N2 119.2(8) . . ?
C4 C5 C6 117.5(11) . . ?
C4 C5 C10 123.3(10) . . ?
C6 C5 C10 119.2(11) . . ?
C7 C6 C5 121.1(12) . . ?
C6 C7 C8 119.7(10) . . ?
C6 C7 C11 121.5(12) . . ?
C8 C7 C11 118.8(12) . . ?
C7 C8 C9 120.7(11) . . ?
C4 C9 C8 118.3(9) . . ?
C4 C9 C12 123.9(9) . . ?
C8 C9 C12 117.7(10) . . ?
N3 C13 N1 113.9(8) . . ?
N4 C14 N3 114.1(9) . . ?
N3 C15 C16 103.4(8) . . ?
N4 C16 C15 102.4(8) . . ?
C18 C17 N4 119.4(9) . . ?
C22 C17 N4 119.0(9) . . ?
C22 C17 C18 121.6(9) . . ?
C17 C18 C19 116.6(10) . . ?
C17 C18 C23 120.9(10) . . ?
C19 C18 C23 122.5(10) . . ?
C20 C19 C18 122.6(10) . . ?
C19 C20 C21 118.6(11) . . ?
C19 C20 C24 120.0(11) . . ?
C21 C20 C24 121.3(11) . . ?
C22 C21 C20 122.6(10) . . ?
C17 C22 C25 121.8(10) . . ?
C21 C22 C17 117.6(10) . . ?
C21 C22 C25 120.6(10) . . ?
N5 C26 C27 173(2) . . ?

_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_16cv001_0m
_database_code_depnum_ccdc_archive 'CCDC 1493770'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_audit_creation_date             2016-04-27
_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         '2(C12 H16 I N2 Pd0.5)'
_chemical_formula_sum            'C24 H32 I2 N4 Pd'
_chemical_formula_weight         736.74
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.8558(2)
_cell_length_b                   11.7308(3)
_cell_length_c                   14.0161(4)
_cell_angle_alpha                68.8980(10)
_cell_angle_beta                 87.9590(10)
_cell_angle_gamma                75.9680(10)
_cell_volume                     1315.74(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.667
_cell_measurement_theta_min      3.385
_exptl_absorpt_coefficient_mu    24.240
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1073 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.4728.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13895
_diffrn_reflns_theta_full        66.67
_diffrn_reflns_theta_max         66.67
_diffrn_reflns_theta_min         3.39
_diffrn_ambient_temperature      99.89
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker AXS PHOTON-100'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       ?
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  
'Bruker multilayer X-ray optics (Goebel mirror)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4408
_reflns_number_total             4599
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.101
_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)+(0.0298P)²+1.9423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_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:
 C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C13(H13), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), 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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
I1 I 0.76667(3) 0.85216(2) 0.092842(17) 0.01916(8) Uani 1 d . . 1 . . .
Pd1 Pd 0.5000 1.0000 0.0000 0.01120(9) Uani 1 d . . 2 S T P
N1 N 0.3974(4) 0.8571(3) 0.0656(2) 0.0151(6) Uani 1 d . . 1 . . .
N2 N 0.3452(4) 0.6687(3) 0.1035(2) 0.0133(6) Uani 1 d . . 1 . . .
C1 C 0.4367(4) 0.7476(3) 0.0580(2) 0.0125(7) Uani 1 d . . 1 . . .
H1 H 0.5249 0.7238 0.0225 0.015 Uiso 1 calc . . 1 R . .
C2 C 0.2591(5) 0.8605(3) 0.1286(3) 0.0210(8) Uani 1 d . . 1 . . .
H2A H 0.1679 0.9258 0.0883 0.025 Uiso 1 calc . . 1 R . .
H2B H 0.2806 0.8789 0.1897 0.025 Uiso 1 calc . . 1 R . .
C3 C 0.2291(5) 0.7295(4) 0.1602(3) 0.0225(8) Uani 1 d . . 1 . . .
H3A H 0.2469 0.6838 0.2351 0.027 Uiso 1 calc . . 1 R . .
H3B H 0.1215 0.7343 0.1392 0.027 Uiso 1 calc . . 1 R . .
C4 C 0.3798(4) 0.5370(3) 0.1232(2) 0.0118(7) Uani 1 d . . 1 . . .
C5 C 0.2790(4) 0.4923(3) 0.0777(3) 0.0155(7) Uani 1 d . . 1 . . .
C6 C 0.3033(4) 0.3624(3) 0.1056(3) 0.0149(7) Uani 1 d . . 1 . . .
H6 H 0.2347 0.3308 0.0769 0.018 Uiso 1 calc . . 1 R . .
C7 C 0.4249(5) 0.2773(3) 0.1742(3) 0.0165(7) Uani 1 d . . 1 . . .
C8 C 0.5265(4) 0.3251(3) 0.2136(3) 0.0157(7) Uani 1 d . . 1 . . .
H8 H 0.6127 0.2681 0.2579 0.019 Uiso 1 calc . . 1 R . .
C9 C 0.5057(4) 0.4543(3) 0.1901(3) 0.0133(7) Uani 1 d . . 1 . . .
C10 C 0.1514(5) 0.5826(4) 0.0016(3) 0.0259(9) Uani 1 d . . 1 . . .
H10A H 0.0605 0.6086 0.0378 0.039 Uiso 1 calc . . 1 GR . .
H10B H 0.1225 0.5416 -0.0423 0.039 Uiso 1 calc . . 1 GR . .
H10C H 0.1874 0.6569 -0.0405 0.039 Uiso 1 calc . . 1 GR . .
C11 C 0.4442(5) 0.1369(3) 0.2055(3) 0.0218(8) Uani 1 d . . 1 . . .
H11A H 0.4080 0.1034 0.2746 0.033 Uiso 1 calc . . 1 GR . .
H11B H 0.5544 0.0957 0.2049 0.033 Uiso 1 calc . . 1 GR . .
H11C H 0.3827 0.1205 0.1573 0.033 Uiso 1 calc . . 1 GR . .
C12 C 0.6131(5) 0.5029(4) 0.2377(3) 0.0229(8) Uani 1 d . . 1 . . .
H12A H 0.6730 0.5500 0.1845 0.034 Uiso 1 calc . . 1 GR . .
H12B H 0.6847 0.4318 0.2891 0.034 Uiso 1 calc . . 1 GR . .
H12C H 0.5516 0.5586 0.2705 0.034 Uiso 1 calc . . 1 GR . .
I2 I 0.23072(3) 0.66198(2) 0.458573(18) 0.02069(9) Uani 1 d . . 1 . . .
Pd2 Pd 0.5000 0.5000 0.5000 0.01066(9) Uani 1 d . . 2 S T P
N3 N 0.3907(4) 0.3617(3) 0.5237(2) 0.0139(6) Uani 1 d . . 1 . . .
N4 N 0.2709(4) 0.2294(3) 0.4932(2) 0.0141(6) Uani 1 d . . 1 . . .
C13 C 0.3580(4) 0.3155(3) 0.4595(3) 0.0132(7) Uani 1 d . . 1 . . .
H13 H 0.3927 0.3400 0.3918 0.016 Uiso 1 calc . . 1 R . .
C14 C 0.3200(5) 0.3034(4) 0.6213(3) 0.0200(8) Uani 1 d . . 1 . . .
H14A H 0.2512 0.3689 0.6429 0.024 Uiso 1 calc . . 1 R . .
H14B H 0.4017 0.2509 0.6763 0.024 Uiso 1 calc . . 1 R . .
C15 C 0.2258(5) 0.2219(4) 0.5975(3) 0.0173(7) Uani 1 d . . 1 . . .
H15A H 0.2550 0.1339 0.6468 0.021 Uiso 1 calc . . 1 R . .
H15B H 0.1123 0.2566 0.5986 0.021 Uiso 1 calc . . 1 R . .
C16 C 0.1874(4) 0.1952(3) 0.4264(3) 0.0140(7) Uani 1 d . . 1 . . .
C17 C 0.0944(4) 0.2888(3) 0.3423(3) 0.0143(7) Uani 1 d . . 1 . . .
C18 C 0.0212(4) 0.2506(3) 0.2774(3) 0.0162(7) Uani 1 d . . 1 . . .
H18 H -0.0403 0.3131 0.2195 0.019 Uiso 1 calc . . 1 R . .
C19 C 0.0345(4) 0.1238(4) 0.2939(3) 0.0174(7) Uani 1 d . . 1 . . .
C20 C 0.1218(5) 0.0344(3) 0.3800(3) 0.0182(8) Uani 1 d . . 1 . . .
H20 H 0.1285 -0.0522 0.3939 0.022 Uiso 1 calc . . 1 R . .
C21 C 0.2002(4) 0.0668(3) 0.4470(3) 0.0158(7) Uani 1 d . . 1 . . .
C22 C 0.0714(5) 0.4278(3) 0.3213(3) 0.0193(8) Uani 1 d . . 1 . . .
H22A H 0.1605 0.4562 0.2859 0.029 Uiso 1 calc . . 1 GR . .
H22B H 0.0634 0.4420 0.3863 0.029 Uiso 1 calc . . 1 GR . .
H22C H -0.0244 0.4752 0.2783 0.029 Uiso 1 calc . . 1 GR . .
C23 C -0.0419(5) 0.0859(4) 0.2194(3) 0.0210(8) Uani 1 d . . 1 . . .
H23A H 0.0105 0.1065 0.1548 0.032 Uiso 1 calc . . 1 GR . .
H23B H -0.1520 0.1317 0.2067 0.032 Uiso 1 calc . . 1 GR . .
H23C H -0.0338 -0.0050 0.2484 0.032 Uiso 1 calc . . 1 GR . .
C24 C 0.2967(5) -0.0354(3) 0.5385(3) 0.0207(8) Uani 1 d . . 1 . . .
H24A H 0.2340 -0.0495 0.5988 0.031 Uiso 1 calc . . 1 GR . .
H24B H 0.3886 -0.0094 0.5514 0.031 Uiso 1 calc . . 1 GR . .
H24C H 0.3299 -0.1136 0.5246 0.031 Uiso 1 calc . . 1 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
I1 Pd1 2.6241(2) . ?
Pd1 I1 2.6241(2) 2_675 ?
Pd1 N1 2.013(3) . ?
Pd1 N1 2.013(3) 2_675 ?
N1 C1 1.289(5) . ?
N1 C2 1.485(5) . ?
N2 C1 1.349(5) . ?
N2 C3 1.480(4) . ?
N2 C4 1.424(4) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.526(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.409(5) . ?
C4 C9 1.399(5) . ?
C5 C6 1.393(5) . ?
C5 C10 1.493(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(5) . ?
C7 C8 1.390(6) . ?
C7 C11 1.511(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.396(5) . ?
C9 C12 1.503(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
I2 Pd2 2.5964(2) . ?
Pd2 I2 2.5964(2) 2_666 ?
Pd2 N3 2.008(3) . ?
Pd2 N3 2.008(3) 2_666 ?
N3 C13 1.279(5) . ?
N3 C14 1.484(5) . ?
N4 C13 1.359(5) . ?
N4 C15 1.479(4) . ?
N4 C16 1.431(5) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.536(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.405(5) . ?
C16 C21 1.404(5) . ?
C17 C18 1.387(5) . ?
C17 C22 1.511(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.396(5) . ?
C19 C20 1.385(6) . ?
C19 C23 1.508(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(5) . ?
C21 C24 1.512(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pd1 I1 180.0 . 2_675 ?
N1 Pd1 I1 90.60(9) . 2_675 ?
N1 Pd1 I1 90.60(9) 2_675 . ?
N1 Pd1 I1 89.40(9) . . ?
N1 Pd1 I1 89.40(9) 2_675 2_675 ?
N1 Pd1 N1 180.0 2_675 . ?
C1 N1 Pd1 126.3(2) . . ?
C1 N1 C2 107.7(3) . . ?
C2 N1 Pd1 126.0(2) . . ?
C1 N2 C3 108.2(3) . . ?
C1 N2 C4 126.6(3) . . ?
C4 N2 C3 122.5(3) . . ?
N1 C1 N2 116.1(3) . . ?
N1 C1 H1 122.0 . . ?
N2 C1 H1 122.0 . . ?
N1 C2 H2A 110.7 . . ?
N1 C2 H2B 110.7 . . ?
N1 C2 C3 105.3(3) . . ?
H2A C2 H2B 108.8 . . ?
C3 C2 H2A 110.7 . . ?
C3 C2 H2B 110.7 . . ?
N2 C3 C2 102.4(3) . . ?
N2 C3 H3A 111.3 . . ?
N2 C3 H3B 111.3 . . ?
C2 C3 H3A 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C5 C4 N2 118.0(3) . . ?
C9 C4 N2 120.6(3) . . ?
C9 C4 C5 121.3(3) . . ?
C4 C5 C10 120.4(3) . . ?
C6 C5 C4 117.9(3) . . ?
C6 C5 C10 121.6(3) . . ?
C5 C6 H6 118.9 . . ?
C5 C6 C7 122.2(3) . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C11 120.7(4) . . ?
C8 C7 C6 118.2(3) . . ?
C8 C7 C11 121.1(3) . . ?
C7 C8 H8 119.0 . . ?
C7 C8 C9 122.0(3) . . ?
C9 C8 H8 119.0 . . ?
C4 C9 C12 120.9(3) . . ?
C8 C9 C4 118.2(3) . . ?
C8 C9 C12 120.8(3) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
I2 Pd2 I2 180.0 2_666 . ?
N3 Pd2 I2 89.09(9) . . ?
N3 Pd2 I2 89.09(9) 2_666 2_666 ?
N3 Pd2 I2 90.91(9) . 2_666 ?
N3 Pd2 I2 90.91(9) 2_666 . ?
N3 Pd2 N3 180.0 2_666 . ?
C13 N3 Pd2 128.3(2) . . ?
C13 N3 C14 108.1(3) . . ?
C14 N3 Pd2 123.4(2) . . ?
C13 N4 C15 107.6(3) . . ?
C13 N4 C16 123.5(3) . . ?
C16 N4 C15 124.2(3) . . ?
N3 C13 N4 116.4(3) . . ?
N3 C13 H13 121.8 . . ?
N4 C13 H13 121.8 . . ?
N3 C14 H14A 110.8 . . ?
N3 C14 H14B 110.8 . . ?
N3 C14 C15 104.8(3) . . ?
H14A C14 H14B 108.9 . . ?
C15 C14 H14A 110.8 . . ?
C15 C14 H14B 110.8 . . ?
N4 C15 C14 102.5(3) . . ?
N4 C15 H15A 111.3 . . ?
N4 C15 H15B 111.3 . . ?
C14 C15 H15A 111.3 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
C17 C16 N4 120.3(3) . . ?
C21 C16 N4 118.7(3) . . ?
C21 C16 C17 121.0(3) . . ?
C16 C17 C22 122.3(3) . . ?
C18 C17 C16 118.0(3) . . ?
C18 C17 C22 119.7(3) . . ?
C17 C18 H18 118.7 . . ?
C17 C18 C19 122.5(3) . . ?
C19 C18 H18 118.7 . . ?
C18 C19 C23 121.0(3) . . ?
C20 C19 C18 117.7(3) . . ?
C20 C19 C23 121.3(3) . . ?
C19 C20 H20 118.8 . . ?
C19 C20 C21 122.4(3) . . ?
C21 C20 H20 118.8 . . ?
C16 C21 C24 121.9(3) . . ?
C20 C21 C16 118.2(3) . . ?
C20 C21 C24 119.9(3) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_olex2_submission_original_sample_id 16cv001
_olex2_submission_special_instructions 'No special instructions were received'
