 
data_p-31c_sq_s
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C284 H330 N54 O88 Pd6' 
_chemical_formula_weight          6546.40

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0147   0.0071
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0257   0.0140
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0407   0.0250
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'   0.0198   3.1361
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            163
_space_group_name_H-M_alt         'P -3 1 c'
_space_group_name_Hall            '-P 3 2c'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 '-y, -x, -z+1/2'
 '-x+y, y, -z+1/2'
 'x, x-y, -z+1/2'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 'y, x, z-1/2'
 'x-y, -y, z-1/2'
 '-x, -x+y, z-1/2'
 
_cell_length_a                    28.7906(4)
_cell_length_b                    28.7906(4)
_cell_length_c                    41.6357(19)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      29888.0(16)
_cell_formula_units_Z             2
_cell_measurement_temperature     100.2(9) 
_cell_measurement_reflns_used     12809
_cell_measurement_theta_min       2.3680
_cell_measurement_theta_max       46.4650
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.727          
_exptl_crystal_F_000              6784
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.2
_exptl_absorpt_coefficient_mu     1.226
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100.2(9) 
_diffrn_radiation_wavelength      1.34050
_diffrn_radiation_type            GaK\a
_diffrn_source                    ?
_diffrn_measurement_device_type    'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             71819
_diffrn_reflns_av_unetI/netI      0.0263
_diffrn_reflns_av_R_equivalents   0.0443
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -31
_diffrn_reflns_limit_k_max        31
_diffrn_reflns_limit_l_min        -45
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.405
_diffrn_reflns_theta_max          46.803
_diffrn_reflns_theta_full         46.803
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              13411
_reflns_number_gt                 6370
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          13411
_refine_ls_number_parameters      613
_refine_ls_number_restraints      598
_refine_ls_R_factor_all           0.2206
_refine_ls_R_factor_gt            0.1695
_refine_ls_wR_factor_ref          0.4816
_refine_ls_wR_factor_gt           0.4232
_refine_ls_goodness_of_fit_ref    1.650
_refine_ls_restrained_S_all       1.670
_refine_ls_shift/su_max           0.015
_refine_ls_shift/su_mean          0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
N1_1 N 0.8411(2) 0.2545(2) 0.44675(19) 0.156(3) Uani 1 1 d G U . . .
C2_1 C 0.8593(2) 0.2631(2) 0.47830(19) 0.147(3) Uani 1 1 d G U . . .
H2_1 H 0.865086 0.237825 0.488706 0.176 Uiso 1 1 calc R U . . .
C3_1 C 0.8690(2) 0.3095(3) 0.49428(15) 0.145(3) Uani 1 1 d G U . . .
H3_1 H 0.881183 0.315237 0.515379 0.173 Uiso 1 1 calc R U . . .
C4_1 C 0.8604(2) 0.3472(2) 0.47872(18) 0.130(3) Uani 1 1 d G U . . .
C5_1 C 0.8421(2) 0.3386(2) 0.44718(18) 0.145(3) Uani 1 1 d G U . . .
H5_1 H 0.836326 0.363842 0.436765 0.173 Uiso 1 1 calc R U . . .
C6_1 C 0.8324(2) 0.2922(3) 0.43119(15) 0.138(3) Uani 1 1 d G U . . .
H6_1 H 0.820228 0.286431 0.410091 0.166 Uiso 1 1 calc R U . . .
C7_1 C 0.8695(3) 0.3963(4) 0.4961(3) 0.128(3) Uani 1 1 d . U . . .
N8_1 N 0.8864(3) 0.4023(3) 0.5253(3) 0.129(2) Uani 1 1 d . U . . .
C9_1 C 0.8950(3) 0.4474(4) 0.5393(3) 0.133(3) Uani 1 1 d . U . . .
N10_1 N 0.8862(3) 0.4837(3) 0.5260(3) 0.130(2) Uani 1 1 d . U . . .
C11_1 C 0.8697(4) 0.4736(4) 0.4962(3) 0.132(3) Uani 1 1 d . U . . .
N12_1 N 0.8600(3) 0.4301(3) 0.4797(2) 0.129(2) Uani 1 1 d . U . . .
N13_1 N 0.8394(3) 0.5845(4) 0.4462(3) 0.154(3) Uani 1 1 d . U . . .
C14_1 C 0.8306(4) 0.5409(4) 0.4317(3) 0.140(3) Uani 1 1 d . U . . .
H14_1 H 0.816773 0.533431 0.410923 0.168 Uiso 1 1 calc R U . . .
C15_1 C 0.8421(4) 0.5056(4) 0.4478(3) 0.146(3) Uani 1 1 d . U . . .
H15_1 H 0.837234 0.475130 0.437024 0.176 Uiso 1 1 calc R U . . .
C16_1 C 0.8594(3) 0.5130(3) 0.4771(3) 0.126(3) Uani 1 1 d . U . . .
C17_1 C 0.8700(3) 0.5623(4) 0.4935(3) 0.142(3) Uani 1 1 d . U . . .
H17_1 H 0.883565 0.570125 0.514344 0.171 Uiso 1 1 calc R U . . .
C18_1 C 0.8591(4) 0.5957(4) 0.4768(3) 0.143(3) Uani 1 1 d . U . . .
H18_1 H 0.865122 0.627416 0.486373 0.172 Uiso 1 1 calc R U . . .
N19_1 N 0.9472(3) 0.4733(4) 0.63530(16) 0.191(4) Uani 1 1 d G U . . .
C20_1 C 0.9394(3) 0.5112(3) 0.6193(2) 0.176(4) Uani 1 1 d DG U . . .
H20_1 H 0.944635 0.541810 0.630057 0.211 Uiso 1 1 calc R U . . .
C21_1 C 0.9236(3) 0.5034(3) 0.5873(2) 0.159(3) Uani 1 1 d G U . . .
H21_1 H 0.918409 0.528799 0.576594 0.191 Uiso 1 1 calc R U . . .
C22_1 C 0.9158(3) 0.4577(4) 0.57124(16) 0.145(3) Uani 1 1 d G U . . .
C23_1 C 0.9236(3) 0.4198(3) 0.5872(2) 0.154(3) Uani 1 1 d G U . . .
H23_1 H 0.918304 0.389175 0.576485 0.185 Uiso 1 1 calc R U . . .
C24_1 C 0.9393(3) 0.4276(3) 0.6193(2) 0.173(4) Uani 1 1 d DG U . . .
H24_1 H 0.944530 0.402185 0.629948 0.208 Uiso 1 1 calc R U . . .
C25_1 C 0.9606(6) 0.4804(6) 0.6707(3) 0.260(7) Uani 1 1 d D U . . .
H25A_1 H 0.991701 0.476539 0.674667 0.312 Uiso 1 1 calc R U . . .
H25B_1 H 0.969139 0.516073 0.677450 0.312 Uiso 1 1 calc R U . . .
C26_1 C 0.9148(5) 0.4402(5) 0.6891(3) 0.350(9) Uani 1 1 d DG U . . .
C27_1 C 0.8648(6) 0.4363(6) 0.6884(3) 0.353(9) Uani 1 1 d DG U . . .
H27_1 H 0.860228 0.462076 0.677582 0.424 Uiso 1 1 calc R U . . .
C28_1 C 0.8215(5) 0.3941(7) 0.7038(4) 0.401(10) Uani 1 1 d DG U . . .
H28_1 H 0.787967 0.391484 0.703359 0.481 Uiso 1 1 calc R U . . .
C29_1 C 0.8282(6) 0.3556(6) 0.7200(4) 0.429(11) Uani 1 1 d DG U . . .
C30_1 C 0.8783(7) 0.3594(6) 0.7207(4) 0.447(11) Uani 1 1 d DG U . . .
H30_1 H 0.882855 0.333699 0.731484 0.536 Uiso 1 1 calc R U . . .
C31_1 C 0.9216(6) 0.4017(6) 0.7052(4) 0.402(10) Uani 1 1 d DG U . . .
H31_1 H 0.955117 0.404291 0.705708 0.482 Uiso 1 1 calc R U . . .
C33_1 C 0.7787(6) 0.2986(7) 0.7685(3) 0.469(15) Uani 1 1 d D U . . .
H33_1 H 0.805094 0.325117 0.781302 0.563 Uiso 1 1 calc R U . . .
C34_1 C 0.7390(8) 0.2527(9) 0.7823(2) 0.493(17) Uani 1 1 d D U . . .
H34_1 H 0.741897 0.243812 0.803345 0.592 Uiso 1 1 calc R U . . .
C32_1 C 0.7799(7) 0.3056(6) 0.7360(3) 0.455(13) Uani 1 1 d D U . . .
O1_2 O 0.3967(5) 0.1983(5) 0.6290(4) 0.262(5) Uani 1 1 d . U . . .
C2_2 C 0.4510(8) 0.2260(8) 0.6177(6) 0.242(5) Uani 1 1 d . U . . .
C3_2 C 0.4821(8) 0.2824(8) 0.6329(6) 0.273(6) Uani 1 1 d . U . . .
H3A_2 H 0.484873 0.279494 0.655958 0.327 Uiso 1 1 calc R U . . .
H3B_2 H 0.463451 0.302118 0.628883 0.327 Uiso 1 1 calc R U . . .
C4_2 C 0.4814(8) 0.2014(8) 0.6321(5) 0.253(5) Uani 1 1 d . U . . .
H4A_2 H 0.461003 0.162904 0.628804 0.303 Uiso 1 1 calc R U . . .
H4B_2 H 0.484172 0.207741 0.655105 0.303 Uiso 1 1 calc R U . . .
C6_2 C 0.5443(9) 0.3150(8) 0.6161(5) 0.260(6) Uani 1 1 d D U . . .
H6_2 H 0.565951 0.351879 0.623899 0.312 Uiso 1 1 calc R U . . .
C5_2 C 0.4542(7) 0.2258(7) 0.5808(5) 0.241(5) Uani 1 1 d D U . . .
H5A_2 H 0.437894 0.189147 0.573114 0.290 Uiso 1 1 calc R U . . .
H5B_2 H 0.434448 0.241860 0.571746 0.290 Uiso 1 1 calc R U . . .
C7_2 C 0.5369(8) 0.3120(7) 0.5815(5) 0.250(6) Uani 1 1 d D U . . .
H7A_2 H 0.571373 0.333531 0.571125 0.300 Uiso 1 1 calc R U . . .
H7B_2 H 0.514264 0.326858 0.575720 0.300 Uiso 1 1 calc R U . . .
C8_2 C 0.5124(7) 0.2571(7) 0.5698(5) 0.247(5) Uani 1 1 d D U . . .
H8_2 H 0.514106 0.256995 0.546281 0.297 Uiso 1 1 calc R U . . .
C9_2 C 0.5345(8) 0.2258(7) 0.5830(5) 0.247(5) Uani 1 1 d . U . . .
H9A_2 H 0.570193 0.239756 0.574178 0.296 Uiso 1 1 calc R U . . .
H9B_2 H 0.512917 0.189370 0.575070 0.296 Uiso 1 1 calc R U . . .
C10_2 C 0.5385(8) 0.2228(8) 0.6184(6) 0.246(5) Uani 1 1 d . U . . .
C11_2 C 0.5667(8) 0.2816(8) 0.6246(6) 0.263(6) Uani 1 1 d . U . . .
H11A_2 H 0.573952 0.286232 0.647500 0.316 Uiso 1 1 calc R U . . .
H11B_2 H 0.601188 0.296758 0.613970 0.316 Uiso 1 1 calc R U . . .
O12_2 O 0.666667 0.333333 0.4120(4) 0.209(6) Uani 1 3 d S TU P . .
C13_2 C 0.666667 0.333333 0.4451(7) 0.179(6) Uani 1 3 d DS TU P . .
C14_2 C 0.6143(6) 0.2889(6) 0.4598(4) 0.267(7) Uani 1 1 d D U . . .
H14A_2 H 0.606446 0.254710 0.450649 0.320 Uiso 1 1 calc R U . . .
H14B_2 H 0.585275 0.295128 0.453915 0.320 Uiso 1 1 calc R U . . .
C15_2 C 0.6160(5) 0.2854(5) 0.4966(4) 0.203(5) Uani 1 1 d D U . . .
H15_2 H 0.583805 0.255072 0.505810 0.243 Uiso 1 1 calc R U . . .
C16_2 C 0.6196(5) 0.3367(5) 0.5017(4) 0.196(4) Uani 1 1 d D U . . .
H16A_2 H 0.593310 0.338277 0.487892 0.235 Uiso 1 1 calc R U . . .
H16B_2 H 0.608846 0.337418 0.523690 0.235 Uiso 1 1 calc R U . . .
N1_3 N 0.7921(5) 0.1105(4) 0.4026(3) 0.202(4) Uani 1 1 d D U . . .
Pd1_3 Pd 0.81734(3) 0.18280(3) 0.42441(3) 0.1622(6) Uani 1 1 d D U . . .
C2_3 C 0.8858(6) 0.1611(6) 0.3872(5) 0.256(6) Uani 1 1 d D U . . .
H2A_3 H 0.900429 0.171094 0.365691 0.307 Uiso 1 1 calc R U . . .
H2B_3 H 0.908929 0.151702 0.399062 0.307 Uiso 1 1 calc R U . . .
C3_3 C 0.8355(6) 0.1153(6) 0.3848(5) 0.253(6) Uani 1 1 d D U . . .
H3A_3 H 0.839771 0.084985 0.390367 0.303 Uiso 1 1 calc R U . . .
H3B_3 H 0.825149 0.111246 0.362370 0.303 Uiso 1 1 calc R U . . .
N4_3 N 0.8889(5) 0.2083(5) 0.4024(4) 0.211(4) Uani 1 1 d D U . . .
C5_3 C 0.7736(8) 0.0650(6) 0.4281(4) 0.242(6) Uani 1 1 d . U . . .
H5A_3 H 0.796557 0.049741 0.427097 0.290 Uiso 1 1 calc R U . . .
H5B_3 H 0.737323 0.037703 0.423686 0.290 Uiso 1 1 calc DR U . . .
H5C_3 H 0.775582 0.079513 0.449118 0.290 Uiso 1 1 calc R U . . .
C6_3 C 0.9037(7) 0.2556(7) 0.3797(5) 0.245(7) Uani 1 1 d . U . . .
H6A_3 H 0.902591 0.244257 0.357939 0.368 Uiso 1 1 calc R U . . .
H6B_3 H 0.939173 0.284135 0.384678 0.368 Uiso 1 1 calc R U . . .
H6C_3 H 0.878594 0.268049 0.382407 0.368 Uiso 1 1 calc R U . . .
C7_3 C 0.9375(6) 0.2295(7) 0.4292(5) 0.232(6) Uani 1 1 d . U . . .
H7A_3 H 0.969759 0.234885 0.419007 0.348 Uiso 1 1 calc R U . . .
H7B_3 H 0.927508 0.203231 0.445923 0.348 Uiso 1 1 calc R U . . .
H7C_3 H 0.943658 0.262764 0.438304 0.348 Uiso 1 1 calc R U . . .
C4_3 C 0.7434(7) 0.0950(6) 0.3788(4) 0.225(6) Uani 1 1 d . U . . .
H4A_3 H 0.753518 0.090691 0.357475 0.338 Uiso 1 1 calc R U . . .
H4B_3 H 0.734449 0.122935 0.378752 0.338 Uiso 1 1 calc R U . . .
H4C_3 H 0.712938 0.061993 0.385641 0.338 Uiso 1 1 calc DR U . . .
N1_4 N 1.0023(12) 0.4337(8) 0.5002(6) 0.487(15) Uani 1 1 d D U . . .
O3_4 O 1.0166(5) 0.4655(7) 0.5248(5) 0.489(15) Uani 1 1 d D U . . .
O2_4 O 0.9804(6) 0.4417(7) 0.4752(5) 0.472(15) Uani 1 1 d D U . . .
O4_4 O 1.0004(5) 0.3881(6) 0.5029(7) 0.502(16) Uani 1 1 d D U . . .
O5_4 O 0.6315(5) 0.0300(4) 0.4296(5) 0.307(8) Uani 1 1 d . . . . .
O6_4 O 0.9322(6) 0.2997(7) 0.5691(5) 0.350(9) Uani 1 1 d . . . . .
O7_4 O 0.9695(5) 0.3694(5) 0.4314(5) 0.349(10) Uani 1 1 d . . . . .
O9_4 O 0.6119(9) 0.3932(9) 0.3906(4) 0.385(11) Uani 1 1 d . . . . .
O8_4 O 0.7697(6) 0.5397(6) 0.3576(3) 0.287(6) Uani 1 1 d . . . . .
O10_4 O 0.3694(6) 0.3014(7) 0.5692(7) 0.396(12) Uani 1 1 d . . . . .
O12_4 O 1.0672(7) 0.588(2) 0.6187(10) 0.83(5) Uani 1 1 d . . . . .
O11_4 O 0.8557(4) 0.7112(4) 0.4969(4) 0.258(6) Uani 1 1 d . . . . .
O13_4 O 1.000000 0.000000 0.3518(13) 0.59(4) Uani 1 3 d S T P . .
O14_4 O 0.8191(10) 0.3366(7) 0.3566(4) 0.380(11) Uani 1 1 d . . . . .
O15_4 O 1.0665(6) 0.4894(12) 0.6106(6) 0.442(17) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
N1_1 C2_1 1.3900 . ?
N1_1 C6_1 1.3900 . ?
N1_1 Pd1_3 2.044(5) . ?
C2_1 C3_1 1.3900 . ?
C3_1 C4_1 1.3900 . ?
C4_1 C5_1 1.3900 . ?
C4_1 C7_1 1.489(12) . ?
C5_1 C6_1 1.3900 . ?
C7_1 N8_1 1.290(12) . ?
C7_1 N12_1 1.323(12) . ?
N8_1 C9_1 1.330(12) . ?
C9_1 N10_1 1.313(12) . ?
C9_1 C22_1 1.429(13) . ?
N10_1 C11_1 1.307(12) . ?
C11_1 N12_1 1.329(12) . ?
C11_1 C16_1 1.532(15) . ?
N13_1 C14_1 1.299(13) . ?
N13_1 C18_1 1.366(13) . ?
N13_1 Pd1_3 2.055(9) 2_655 ?
C14_1 C15_1 1.392(14) . ?
C15_1 C16_1 1.294(13) . ?
C16_1 C17_1 1.463(13) . ?
C17_1 C18_1 1.346(13) . ?
N19_1 C20_1 1.3900 . ?
N19_1 C24_1 1.3900 . ?
N19_1 C25_1 1.512(15) . ?
C20_1 C21_1 1.3900 . ?
C21_1 C22_1 1.3900 . ?
C22_1 C23_1 1.3900 . ?
C23_1 C24_1 1.3900 . ?
C25_1 C26_1 1.462(14) . ?
C26_1 C27_1 1.3900 . ?
C26_1 C31_1 1.3900 . ?
C27_1 C28_1 1.3900 . ?
C28_1 C29_1 1.3900 . ?
C29_1 C30_1 1.3900 . ?
C29_1 C32_1 1.565(12) . ?
C30_1 C31_1 1.3900 . ?
C33_1 C32_1 1.365(10) . ?
C33_1 C34_1 1.368(10) . ?
C34_1 C32_1 1.379(7) 4_666 ?
O1_2 C2_2 1.43(2) . ?
C2_2 C4_2 1.50(2) . ?
C2_2 C5_2 1.54(2) . ?
C2_2 C3_2 1.55(3) . ?
C3_2 C6_2 1.70(3) . ?
C4_2 C10_2 1.55(2) . ?
C6_2 C11_2 1.44(3) . ?
C6_2 C7_2 1.455(15) . ?
C5_2 C8_2 1.524(16) . ?
C7_2 C8_2 1.455(15) . ?
C8_2 C9_2 1.45(2) . ?
C9_2 C10_2 1.48(2) . ?
C10_2 C11_2 1.49(2) . ?
O12_2 C13_2 1.38(2) . ?
C13_2 C14_2 1.536(13) . ?
C13_2 C14_2 1.536(13) 2_655 ?
C13_2 C14_2 1.536(13) 3_665 ?
C14_2 C15_2 1.537(15) . ?
C15_2 C16_2 1.414(12) 2_655 ?
C15_2 C16_2 1.445(12) . ?
N1_3 C3_3 1.400(15) . ?
N1_3 C5_3 1.557(18) . ?
N1_3 C4_3 1.588(17) . ?
N1_3 Pd1_3 2.041(10) . ?
Pd1_3 N4_3 2.026(10) . ?
C2_3 C3_3 1.391(14) . ?
C2_3 N4_3 1.463(15) . ?
N4_3 C6_3 1.531(18) . ?
N4_3 C7_3 1.65(2) . ?
N1_4 O4_4 1.290(13) . ?
N1_4 O3_4 1.295(13) . ?
N1_4 O2_4 1.298(13) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2_1 N1_1 C6_1 120.0 . . ?
C2_1 N1_1 Pd1_3 121.1(4) . . ?
C6_1 N1_1 Pd1_3 118.5(4) . . ?
N1_1 C2_1 C3_1 120.0 . . ?
C4_1 C3_1 C2_1 120.0 . . ?
C5_1 C4_1 C3_1 120.0 . . ?
C5_1 C4_1 C7_1 120.0(7) . . ?
C3_1 C4_1 C7_1 120.0(7) . . ?
C4_1 C5_1 C6_1 120.0 . . ?
C5_1 C6_1 N1_1 120.0 . . ?
N8_1 C7_1 N12_1 126.2(10) . . ?
N8_1 C7_1 C4_1 117.4(10) . . ?
N12_1 C7_1 C4_1 116.4(11) . . ?
C7_1 N8_1 C9_1 114.5(10) . . ?
N10_1 C9_1 N8_1 125.3(12) . . ?
N10_1 C9_1 C22_1 117.1(11) . . ?
N8_1 C9_1 C22_1 117.6(11) . . ?
C11_1 N10_1 C9_1 114.5(10) . . ?
N10_1 C11_1 N12_1 125.6(11) . . ?
N10_1 C11_1 C16_1 120.7(10) . . ?
N12_1 C11_1 C16_1 113.7(11) . . ?
C7_1 N12_1 C11_1 113.8(10) . . ?
C14_1 N13_1 C18_1 121.3(10) . . ?
C14_1 N13_1 Pd1_3 119.5(9) . 2_655 ?
C18_1 N13_1 Pd1_3 119.0(8) . 2_655 ?
N13_1 C14_1 C15_1 118.7(12) . . ?
C16_1 C15_1 C14_1 123.1(11) . . ?
C15_1 C16_1 C17_1 118.6(10) . . ?
C15_1 C16_1 C11_1 124.5(10) . . ?
C17_1 C16_1 C11_1 116.8(11) . . ?
C18_1 C17_1 C16_1 116.1(11) . . ?
C17_1 C18_1 N13_1 122.2(10) . . ?
C20_1 N19_1 C24_1 120.0 . . ?
C20_1 N19_1 C25_1 119.4(6) . . ?
C24_1 N19_1 C25_1 120.5(6) . . ?
C21_1 C20_1 N19_1 120.0 . . ?
C20_1 C21_1 C22_1 120.0 . . ?
C21_1 C22_1 C23_1 120.0 . . ?
C21_1 C22_1 C9_1 119.8(8) . . ?
C23_1 C22_1 C9_1 119.9(8) . . ?
C24_1 C23_1 C22_1 120.0 . . ?
C23_1 C24_1 N19_1 120.0 . . ?
C26_1 C25_1 N19_1 109.6(8) . . ?
C27_1 C26_1 C31_1 120.0 . . ?
C27_1 C26_1 C25_1 122.7(7) . . ?
C31_1 C26_1 C25_1 117.0(7) . . ?
C26_1 C27_1 C28_1 120.0 . . ?
C27_1 C28_1 C29_1 120.0 . . ?
C30_1 C29_1 C28_1 120.0 . . ?
C30_1 C29_1 C32_1 118.3(7) . . ?
C28_1 C29_1 C32_1 121.6(7) . . ?
C31_1 C30_1 C29_1 120.0 . . ?
C30_1 C31_1 C26_1 120.0 . . ?
C32_1 C33_1 C34_1 120.3(6) . . ?
C33_1 C34_1 C32_1 118.1(8) . 4_666 ?
C33_1 C32_1 C34_1 117.0(8) . 4_666 ?
C33_1 C32_1 C29_1 120.2(9) . . ?
C34_1 C32_1 C29_1 120.0(10) 4_666 . ?
O1_2 C2_2 C4_2 109.8(18) . . ?
O1_2 C2_2 C5_2 112.1(18) . . ?
C4_2 C2_2 C5_2 110.4(17) . . ?
O1_2 C2_2 C3_2 110.3(17) . . ?
C4_2 C2_2 C3_2 99.4(19) . . ?
C5_2 C2_2 C3_2 114.1(18) . . ?
C2_2 C3_2 C6_2 107.9(16) . . ?
C2_2 C4_2 C10_2 114.7(18) . . ?
C11_2 C6_2 C7_2 108(2) . . ?
C11_2 C6_2 C3_2 103.3(18) . . ?
C7_2 C6_2 C3_2 107.0(19) . . ?
C8_2 C5_2 C2_2 110.4(18) . . ?
C6_2 C7_2 C8_2 111.8(18) . . ?
C9_2 C8_2 C7_2 115.2(18) . . ?
C9_2 C8_2 C5_2 102.3(16) . . ?
C7_2 C8_2 C5_2 109.5(17) . . ?
C8_2 C9_2 C10_2 119.0(19) . . ?
C9_2 C10_2 C11_2 97.0(19) . . ?
C9_2 C10_2 C4_2 107.0(18) . . ?
C11_2 C10_2 C4_2 104.8(17) . . ?
C6_2 C11_2 C10_2 122.9(19) . . ?
O12_2 C13_2 C14_2 113.5(12) . . ?
O12_2 C13_2 C14_2 113.6(12) . 2_655 ?
C14_2 C13_2 C14_2 105.1(13) . 2_655 ?
O12_2 C13_2 C14_2 113.6(12) . 3_665 ?
C14_2 C13_2 C14_2 105.1(13) . 3_665 ?
C14_2 C13_2 C14_2 105.1(13) 2_655 3_665 ?
C13_2 C14_2 C15_2 113.7(16) . . ?
C16_2 C15_2 C16_2 116.7(13) 2_655 . ?
C16_2 C15_2 C14_2 102.6(12) 2_655 . ?
C16_2 C15_2 C14_2 93.9(12) . . ?
C15_2 C16_2 C15_2 118.8(12) 3_665 . ?
C3_3 N1_3 C5_3 110.8(13) . . ?
C3_3 N1_3 C4_3 108.3(14) . . ?
C5_3 N1_3 C4_3 107.9(11) . . ?
C3_3 N1_3 Pd1_3 106.8(7) . . ?
C5_3 N1_3 Pd1_3 110.7(9) . . ?
C4_3 N1_3 Pd1_3 112.3(7) . . ?
N4_3 Pd1_3 N1_3 87.1(5) . . ?
N4_3 Pd1_3 N1_1 94.2(3) . . ?
N1_3 Pd1_3 N1_1 178.7(4) . . ?
N4_3 Pd1_3 N13_1 177.1(4) . 3_665 ?
N1_3 Pd1_3 N13_1 95.2(4) . 3_665 ?
N1_1 Pd1_3 N13_1 83.6(3) . 3_665 ?
C3_3 C2_3 N4_3 117.5(9) . . ?
C2_3 C3_3 N1_3 120.8(9) . . ?
C2_3 N4_3 C6_3 114.9(14) . . ?
C2_3 N4_3 C7_3 106.4(13) . . ?
C6_3 N4_3 C7_3 106.3(12) . . ?
C2_3 N4_3 Pd1_3 106.3(7) . . ?
C6_3 N4_3 Pd1_3 112.5(8) . . ?
C7_3 N4_3 Pd1_3 110.4(9) . . ?
O4_4 N1_4 O3_4 119.1(13) . . ?
O4_4 N1_4 O2_4 118.3(13) . . ?
O3_4 N1_4 O2_4 121.3(13) . . ?
 
_refine_diff_density_max    2.389
_refine_diff_density_min   -0.557
_refine_diff_density_rms    0.145




# start Validation Reply Form
_vrf_THETM01_p-31c_sq_s
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals of this giant supramolecular assembly is very poorly 
diffracting£¬possibly due to a large amount of amorphous solvents and 
highly-disordered counterions existing in the unit cell, which occupy as
 much as 60% of the unit cell based on PLATON calculation.
;
_vrf_PLAT084_p-31c_sq_s
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.48 Report
RESPONSE: The refinement model is poor because the p-terphenyl group in the crystal
structure may be disorder and arrange in two directions.
;
# end Validation Reply Form

