 
data_MARMON138B_SQn
# start Validation Reply Form
_vrf_PLAT082_MARMON138B_SQn
;
PROBLEM: High R1 Value ..................................       0.31 Report
RESPONSE: the quality of the SCXRD data did not allow the precision for the complete visualization of crystal structure and in situ generated supramolecular metal clusters
;
_vrf_PLAT084_MARMON138B_SQn
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.69 Report
RESPONSE: low precision in model as explained in details at supporting info of the paper. 
;
_vrf_PLAT213_MARMON138B_SQn
;
PROBLEM: Atom N1              has ADP max/min Ratio .....        5.4 prolat
RESPONSE: severe disorder
;
_vrf_PLAT260_MARMON138B_SQn
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PROBLEM: Large Average Ueq of Residue Including       Cu1      0.334 Check 
RESPONSE: severe disorder
;
_vrf_PLAT307_MARMON138B_SQn
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PROBLEM: Isolated Metal Atom found in Structure (Unusual)        Au2 Check 
RESPONSE: bounded organic fragments are severely disordered and not detected  
;
_vrf_PLAT412_MARMON138B_SQn
;
PROBLEM: Short Intra XH3 .. XHn     H12B     ..H12B     .       1.53 Ang.  
RESPONSE: thermal disorder of dynamic fragments residing in huge pores
;
_vrf_PLAT430_MARMON138B_SQn
;
PROBLEM: Short Inter D...A Contact  N6L      ..O6W      .       2.22 Ang.  
RESPONSE: The distance suggests a strong Hydrogen bond, the highly disordered water occupying so huge pores may be at the origin of a so short value that, of course, must be considered as an averaged situation in the crystal via only one unit cell. 
;
_vrf_PLAT026_MARMON138B_SQn
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PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        33% Check 
RESPONSE: expected in porous structures
;
_vrf_PLAT201_MARMON138B_SQn
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PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          2 Report
RESPONSE: severe disorder
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_vrf_PLAT241_MARMON138B_SQn
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PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        Cu1 Check 
RESPONSE: thermal disorder
;
_vrf_PLAT242_MARMON138B_SQn
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cu2 Check 
RESPONSE: disorder
;
_vrf_PLAT250_MARMON138B_SQn
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        6.3 Note  
RESPONSE: severe disorder
;
_vrf_PLAT306_MARMON138B_SQn
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W Check 
RESPONSE: normal in a so vastly nano-space 
;
_vrf_PLAT315_MARMON138B_SQn
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).        C3S Check 
RESPONSE: isolated fragment, the bounded atoms are severely disordered and not defined
;
_vrf_PLAT342_MARMON138B_SQn
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02283 Ang.  
RESPONSE: poor precision due to quality of crystal that suffered two consecutive sc-sc trasformations
;
_vrf_PLAT934_MARMON138B_SQn
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          4 Check 
RESPONSE: Unavoidable mismatch after a SC to SC process
;
_vrf_PLAT990_MARMON138B_SQn
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note  
RESPONSE: No ABIN command, but all details have been reported
;
# end Validation Reply Form
 
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C101 H174 Au2 Cl3 Cu6 N20 Ni4 O77.50 Pd2 S' 
_chemical_formula_weight          4269.81

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0029   0.0015
 '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'   0.0057   0.0031
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0101   0.0057
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3437   1.0558
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cu'  'Cu'   0.3319   1.2017
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'  -1.0531   0.9556
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Au'  'Au'  -1.6328   8.3932
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1139   0.1106
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            123
_space_group_name_H-M_alt         'P 4/m m m'
_space_group_name_Hall            '-P 4 2'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 '-x, y, -z'
 'x, -y, -z'
 'y, x, -z'
 '-y, -x, -z'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z'
 '-y, x, -z'
 'x, -y, z'
 '-x, y, z'
 '-y, -x, z'
 'y, x, z'
 
_cell_length_a                    35.725(2)
_cell_length_b                    35.725(2)
_cell_length_c                    15.2666(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      19485(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     30(2)
_cell_measurement_reflns_used     26353
_cell_measurement_theta_max       33.9117683767
_cell_measurement_theta_min       0.550453324127

 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.456          
_exptl_crystal_F_000              8572
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.06 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.05 
_exptl_absorpt_coefficient_mu     2.506
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_T_min   0.980870699954
_exptl_absorpt_correction_T_max   1.0
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_process_details    
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;

 
_diffrn_ambient_temperature       30(2)
_diffrn_radiation_wavelength      0.6889
_diffrn_detector                  'Photon counting pixel array'
_diffrn_radiation_type            Synchrotron
_diffrn_measurement_device        'data_PILATUS_2M_S_N_24_0107_Diamond'
_diffrn_measurement_device_type   'Fluid Film Devices'
_diffrn_measurement_method        'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_source          'Diamond Light Source Beamline I19-1'
_diffrn_radiation_monochromator   'Silicon 111'
_diffrn_reflns_number             244768
_diffrn_reflns_av_unetI/netI      0.0877
_diffrn_reflns_av_R_equivalents   0.1736
_diffrn_reflns_limit_h_min        -43
_diffrn_reflns_limit_h_max        43
_diffrn_reflns_limit_k_min        -43
_diffrn_reflns_limit_k_max        43
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          0.552
_diffrn_reflns_theta_max          25.000
_diffrn_reflns_theta_full         24.415
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              10377
_reflns_number_gt                 3377
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_audit_creation_method            'XIA2 0.5.542-g41349194-dials-1.9'
_audit_creation_date              2018-04-16
_computing_data_reduction         
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.9.1-g449277ff-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.542-g41349194-dials-1.9 (Winter, G., 2010)
;

_publ_section_references          
;
Evans, P. (2006) Acta Cryst. D62, 72-82.
Evans, P. R. and Murshudov, G. N. (2013) Acta Cryst. D69, 1204-1214.
Winn, M. D. et al. (2011) Acta Cryst. D67, 235-242.
Winter, G. (2010) J. Appl. Cryst. 43, 186-190.
Winter, G. et al. (2018) Acta Cryst. D74, 85-97.
;
 
_computing_cell_refinement        'DIALS 2theta refinement, DIALS 1.9.1-g449277ff-release'
_computing_structure_solution     'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'CRYSTAL MAKER'
_computing_publication_material   'Bruker SHELXTL'
 
_refine_special_details
;
The quality of the SCXRD data did not allow the complete visualization of SMCs crystal structure. However, many local maxima attributable to Pd2+ and Au3+ metal ions in the channels together with few peaks related to L3 ligands fragments were located in the observed structure factor Fourier maps, providing evidence of the localization of the SMCs. More details are givin in experimental section of the paper.
;
_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+0.5000P] 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          10377
_refine_ls_number_parameters      221
_refine_ls_number_restraints      113
_refine_ls_R_factor_all           0.4234
_refine_ls_R_factor_gt            0.3098
_refine_ls_wR_factor_ref          0.6865
_refine_ls_wR_factor_gt           0.6579
_refine_ls_goodness_of_fit_ref    1.911
_refine_ls_restrained_S_all       2.021
_refine_ls_shift/su_max           0.055
_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
Cu1 Cu 0.2586(3) 0.7414(3) 0.7314(3) 0.399(7) Uani 1 2 d S T P . .
Cu2 Cu 0.5000 0.82756(14) 0.77133(19) 0.253(3) Uani 1 2 d S T P . .
Cu3 Cu 0.35253(8) 1.0000 0.7657(2) 0.196(2) Uani 1 2 d S T P . .
Ni1 Ni 0.35722(17) 0.84998(18) 0.75040(17) 0.327(4) Uani 1 1 d D . . . .
N1 N 0.3122(8) 0.7647(7) 0.6664(9) 0.420(15) Uani 1 1 d D . . . .
N2 N 0.4401(8) 0.8104(6) 0.8414(9) 0.420(15) Uani 1 1 d D . . . .
N3 N 0.3611(6) 0.9477(6) 0.8304(8) 0.420(15) Uani 1 1 d D . . . .
O1 O 0.3629(5) 0.8945(5) 0.8334(9) 0.304(5) Uani 1 1 d D . . . .
O2 O 0.3266(6) 0.8968(6) 0.6820(9) 0.304(5) Uani 1 1 d D . . . .
O3 O 0.3279(6) 0.9557(6) 0.6923(8) 0.304(5) Uani 1 1 d D . . . .
O4 O 0.3903(6) 0.8200(5) 0.8297(8) 0.304(5) Uani 1 1 d D . . . .
O5 O 0.4058(6) 0.8639(5) 0.6851(9) 0.304(5) Uani 1 1 d D . . . .
O6 O 0.4603(6) 0.8523(6) 0.7009(9) 0.304(5) Uani 1 1 d D . . . .
O7 O 0.3400(5) 0.8082(6) 0.6660(9) 0.304(5) Uani 1 1 d D . . . .
O8 O 0.3077(5) 0.8326(5) 0.8023(9) 0.304(5) Uani 1 1 d D . . . .
O9 O 0.2748(6) 0.7869(5) 0.8127(9) 0.304(5) Uani 1 1 d D . . . .
C1 C 0.3521(4) 0.9201(7) 0.7904(10) 0.345(7) Uani 1 1 d D . . . .
C2 C 0.3352(5) 0.9250(6) 0.7204(12) 0.345(7) Uani 1 1 d D . . . .
C3 C 0.3158(5) 0.7932(6) 0.7079(10) 0.345(7) Uani 1 1 d D . . . .
C4 C 0.2991(5) 0.8027(5) 0.7728(9) 0.345(7) Uani 1 1 d D . . . .
C5 C 0.4196(7) 0.8274(4) 0.7953(10) 0.345(7) Uani 1 1 d D . . . .
C6 C 0.4292(7) 0.8472(4) 0.7289(9) 0.345(7) Uani 1 1 d D . . . .
C7 C 0.30816(18) 0.75511(19) 0.5853(10) 0.345(7) Uani 1 1 d D . . . .
C8 C 0.3349(4) 0.7276(4) 0.5802(11) 0.345(7) Uani 1 1 d D . . . .
C9 C 0.3476(4) 0.7145(4) 0.5000 0.345(7) Uani 1 2 d DS T P . .
H9 H 0.3661 0.6955 0.5000 0.413 Uiso 1 2 calc R U P . .
C10 C 0.29862(15) 0.76494(15) 0.5000 0.345(7) Uani 1 2 d DS T P . .
C11 C 0.2686(3) 0.7959(3) 0.5000 0.345(7) Uani 1 2 d DS T P . .
H11A H 0.2455 0.7863 0.5267 0.517 Uiso 0.5 1 calc R U P . .
H11B H 0.2634 0.8036 0.4396 0.517 Uiso 0.5 1 calc R U P . .
H11C H 0.2776 0.8174 0.5336 0.517 Uiso 0.5 1 calc R U P . .
C12 C 0.3520(8) 0.7100(8) 0.6622(13) 0.345(7) Uani 1 1 d D . . . .
H12A H 0.3706 0.6912 0.6449 0.517 Uiso 1 1 calc R U . . .
H12B H 0.3323 0.6980 0.6968 0.517 Uiso 1 1 calc R U . . .
H12C H 0.3642 0.7294 0.6974 0.517 Uiso 1 1 calc R U . . .
C13 C 0.4477(5) 0.7944(8) 0.9108(10) 0.345(7) Uani 1 1 d D . . . .
C14 C 0.44616(19) 0.7550(8) 0.9170(10) 0.345(7) Uani 1 1 d D . . . .
C15 C 0.44557(15) 0.7394(10) 1.0000 0.345(7) Uani 1 2 d DS T P . .
H15 H 0.4446 0.7128 1.0000 0.413 Uiso 1 2 calc R U P . .
C16 C 0.4478(6) 0.7986(14) 1.0000 0.345(7) Uani 1 2 d DS T P . .
C17 C 0.4494(10) 0.8417(14) 1.0000 0.345(7) Uani 1 2 d DS T P . .
H17A H 0.4500 0.8508 1.0605 0.517 Uiso 0.5 1 calc R U P . .
H17B H 0.4273 0.8517 0.9701 0.517 Uiso 0.5 1 calc R U P . .
H17C H 0.4721 0.8500 0.9694 0.517 Uiso 0.5 1 calc R U P . .
C18 C 0.44540(17) 0.7349(9) 0.8247(12) 0.345(7) Uani 1 1 d D . . . .
H18A H 0.4438 0.7077 0.8331 0.517 Uiso 1 1 calc R U . . .
H18B H 0.4683 0.7410 0.7924 0.517 Uiso 1 1 calc R U . . .
H18C H 0.4236 0.7435 0.7914 0.517 Uiso 1 1 calc R U . . .
C19 C 0.38289(11) 0.95068(2) 0.9186(10) 0.345(7) Uani 1 1 d D . . . .
C20 C 0.42164(5) 0.95531(2) 0.9172(9) 0.345(7) Uani 1 1 d D . . . .
C21 C 0.4357(6) 0.95699(7) 1.0000 0.345(7) Uani 1 2 d DS T P . .
H21 H 0.4621 0.9601 1.0000 0.413 Uiso 1 2 calc R U P . .
C22 C 0.3658(5) 0.94864(6) 1.0000 0.345(7) Uani 1 2 d DS T P . .
C23 C 0.3232(7) 0.94355(9) 1.0000 0.345(7) Uani 1 2 d DS T P . .
H23A H 0.3142 0.9422 1.0605 0.517 Uiso 0.5 1 calc R U P . .
H23B H 0.3168 0.9203 0.9693 0.517 Uiso 0.5 1 calc R U P . .
H23C H 0.3115 0.9648 0.9702 0.517 Uiso 0.5 1 calc R U P . .
C24 C 0.44918(8) 0.95860(2) 0.8393(12) 0.345(7) Uani 1 1 d D . . . .
H24A H 0.4746 0.9622 0.8615 0.517 Uiso 1 1 calc R U . . .
H24B H 0.4421 0.9800 0.8027 0.517 Uiso 1 1 calc R U . . .
H24C H 0.4482 0.9356 0.8042 0.517 Uiso 1 1 calc R U . . .
O1W O 0.2867(5) 0.7133(5) 0.8473(17) 0.235(9) Uani 1 2 d S TU P . .
O2W O 0.5000 0.7751(18) 0.671(4) 0.47(3) Uiso 1 2 d S . P . .
O3W O 0.3956(5) 1.0000 0.6704(12) 0.161(6) Uiso 1 2 d S . P . .
O4W O 0.5000 0.8259(11) 0.5000 0.236(13) Uiso 1 4 d S . P . .
O5W O 0.2305(17) 1.0000 0.725(3) 0.45(3) Uiso 1 2 d S . P . .
Pd1 Pd 0.2538(7) 0.8277(9) 0.0000 0.410(11) Uiso 0.5 2 d DS . P . .
Pd2 Pd 0.3291(6) 0.8957(6) 0.5000 0.410(11) Uiso 0.5 2 d DS . P . .
N1L N 0.3029(10) 0.8613(12) 0.0000 0.182(16) Uiso 0.5 2 d DS . P . .
O2L O 0.2030(14) 0.7970(14) 0.0000 0.41(3) Uiso 1 4 d DS . P . .
N3L N 0.2020(13) 0.8557(15) 0.0000 0.38(5) Uiso 0.5 2 d DS . P . .
N4L N 0.2703(9) 0.7713(9) 0.0000 0.597 Uiso 0.5 2 d DS U P . .
N5L N 0.3371(9) 0.8404(6) 0.5000 0.26(3) Uiso 0.5 2 d DS . P . .
N6L N 0.3854(5) 0.9045(6) 0.5000 0.168 Uiso 1 2 d DS U P . .
N7L N 0.2735(6) 0.8896(10) 0.5000 0.175(16) Uiso 0.5 2 d DS . P . .
N8L N 0.3253(8) 0.9512(7) 0.5000 0.354 Uiso 0.5 2 d DS U P . .
Au1 Au 0.4692(4) 1.0704(4) 0.5000 0.529(7) Uiso 0.5 2 d S . P . .
Au2 Au 0.1246(7) 0.8754(7) 0.7583(12) 0.588(2) Uiso 0.5 2 d DS . P . .
S1 S 0.1610(5) 0.9196(5) 0.6838(11) 0.131(5) Uiso 0.25 1 d D . P . .
C3S C 0.193(3) 0.919(3) 0.589(5) 0.235 Uiso 0.25 1 d D U P . .
C2S C 0.209(2) 0.862(3) 0.627(6) 0.288 Uiso 0.25 1 d D U P . .
C1S C 0.1674(13) 0.8743(13) 0.626(6) 0.274 Uiso 0.25 1 d D U P . .
O1S O 0.2283(6) 0.8362(6) 0.5692(6) 0.060(6) Uiso 0.25 1 d D . P . .
O6W O 0.4308(7) 1.0804(7) 0.5931(17) 0.074(7) Uiso 0.25 1 d . . P . .
O7W O 0.5000 1.1012(7) 0.4005(17) 0.124(8) Uiso 0.5 2 d S . P . .
O8W O 0.5000 1.0468(15) 0.378(4) 0.24(2) Uiso 0.5 2 d S . 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
Cu1 O9 2.125(16) 15_665 ?
Cu1 O9 2.125(16) . ?
Cu1 N1 2.31(2) . ?
Cu1 N1 2.31(2) 15_665 ?
Cu1 O1W 2.27(3) . ?
Cu2 O6 1.99(2) 14_655 ?
Cu2 O6 1.99(2) . ?
Cu2 N2 2.47(2) 14_655 ?
Cu2 N2 2.47(2) . ?
Cu3 N3 2.137(19) 13_575 ?
Cu3 N3 2.137(19) . ?
Cu3 O3W 2.118(18) . ?
Cu3 O3 2.129(17) 13_575 ?
Cu3 O3 2.129(17) . ?
Ni1 O4 2.004(16) . ?
Ni1 O8 2.034(14) . ?
Ni1 O7 2.066(17) . ?
Ni1 O1 2.044(17) . ?
Ni1 O5 2.06(2) . ?
Ni1 O2 2.26(3) . ?
Ni1 C5 2.47(3) . ?
N1 C3 1.208(10) . ?
N1 C7 1.29(2) . ?
N2 C13 1.23(3) . ?
N2 C5 1.183(17) . ?
N2 O4 1.82(3) . ?
N3 C1 1.204(17) . ?
N3 C19 1.559(16) . ?
O1 C1 1.187(16) . ?
O2 C2 1.206(16) . ?
O3 C2 1.209(17) . ?
O4 C5 1.199(17) . ?
O5 C6 1.226(16) . ?
O6 C6 1.205(13) . ?
O7 C3 1.201(9) . ?
O8 C4 1.199(9) . ?
O9 C4 1.201(9) . ?
C1 C2 1.239(16) . ?
C3 C4 1.207(9) . ?
C5 C6 1.283(15) . ?
C7 C10 1.391(15) . ?
C7 C8 1.371(18) . ?
C8 C9 1.388(15) . ?
C8 C12 1.530(18) . ?
C9 C8 1.388(15) 10_556 ?
C10 C7 1.391(15) 10_556 ?
C10 C11 1.541(12) . ?
C13 C16 1.369(15) . ?
C13 C14 1.413(17) . ?
C14 C15 1.385(15) . ?
C14 C18 1.581(17) . ?
C15 C14 1.385(15) 10_557 ?
C16 C13 1.369(15) 10_557 ?
C16 C17 1.541(19) . ?
C19 C22 1.385(14) . ?
C19 C20 1.394(4) . ?
C20 C21 1.362(14) . ?
C20 C24 1.548(14) . ?
C21 C20 1.362(15) 10_557 ?
C22 C19 1.385(14) 10_557 ?
C22 C23 1.533(19) . ?
Pd1 N4L 2.10(2) . ?
Pd1 N3L 2.10(2) . ?
Pd1 O2L 2.122(17) . ?
Pd1 N1L 2.124(19) . ?
Pd2 N5L 1.998(17) . ?
Pd2 N8L 1.984(17) . ?
Pd2 N7L 2.000(17) . ?
Pd2 N6L 2.035(16) . ?
O2L Pd1 2.122(17) 15_665 ?
Au1 O6W 2.01(3) . ?
Au1 O6W 2.01(3) 10_556 ?
Au1 Au1 2.20(3) 5_656 ?
Au1 O8W 2.32(5) 10_556 ?
Au1 O8W 2.32(5) . ?
Au1 O7W 2.17(2) 10_556 ?
Au1 O7W 2.17(2) . ?
Au2 S1 2.339(14) 15_665 ?
Au2 S1 2.340(14) . ?
Au2 C1S 2.53(6) 15_665 ?
Au2 C1S 2.53(6) . ?
S1 C3S 1.85(2) . ?
S1 C1S 1.86(2) . ?
C2S O1S 1.46(2) . ?
C2S C1S 1.54(2) . ?
O7W Au1 2.17(2) 5_656 ?
O8W Au1 2.32(5) 5_656 ?
 
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
O9 Cu1 O9 94.4(9) 15_665 . ?
O9 Cu1 N1 169.2(6) 15_665 . ?
O9 Cu1 N1 75.5(6) . . ?
O9 Cu1 N1 75.5(6) 15_665 15_665 ?
O9 Cu1 N1 169.2(6) . 15_665 ?
N1 Cu1 N1 114.3(11) . 15_665 ?
O9 Cu1 O1W 76.3(7) 15_665 . ?
O9 Cu1 O1W 76.3(7) . . ?
N1 Cu1 O1W 97.3(7) . . ?
N1 Cu1 O1W 97.3(7) 15_665 . ?
O6 Cu2 O6 91.1(10) 14_655 . ?
O6 Cu2 N2 74.1(8) 14_655 14_655 ?
O6 Cu2 N2 164.4(8) . 14_655 ?
O6 Cu2 N2 164.4(8) 14_655 . ?
O6 Cu2 N2 74.1(8) . . ?
N2 Cu2 N2 120.1(11) 14_655 . ?
N3 Cu3 N3 122.1(9) 13_575 . ?
N3 Cu3 O3W 102.3(6) 13_575 . ?
N3 Cu3 O3W 102.3(6) . . ?
N3 Cu3 O3 69.7(7) 13_575 13_575 ?
N3 Cu3 O3 162.3(9) . 13_575 ?
O3W Cu3 O3 86.5(6) . 13_575 ?
N3 Cu3 O3 162.3(9) 13_575 . ?
N3 Cu3 O3 69.7(7) . . ?
O3W Cu3 O3 86.5(6) . . ?
O3 Cu3 O3 95.9(11) 13_575 . ?
O4 Ni1 O8 96.6(8) . . ?
O4 Ni1 O7 99.6(8) . . ?
O8 Ni1 O7 76.4(7) . . ?
O4 Ni1 O1 89.1(7) . . ?
O8 Ni1 O1 94.7(7) . . ?
O7 Ni1 O1 168.1(9) . . ?
O4 Ni1 O5 85.6(9) . . ?
O8 Ni1 O5 173.3(6) . . ?
O7 Ni1 O5 97.0(6) . . ?
O1 Ni1 O5 91.7(7) . . ?
O4 Ni1 O2 164.4(6) . . ?
O8 Ni1 O2 89.1(8) . . ?
O7 Ni1 O2 95.9(7) . . ?
O1 Ni1 O2 76.0(7) . . ?
O5 Ni1 O2 90.4(7) . . ?
O4 Ni1 C5 28.8(5) . . ?
O8 Ni1 C5 125.2(7) . . ?
O7 Ni1 C5 101.9(7) . . ?
O1 Ni1 C5 89.6(6) . . ?
O5 Ni1 C5 56.8(6) . . ?
O2 Ni1 C5 144.1(6) . . ?
C3 N1 C7 137.5(15) . . ?
C3 N1 Cu1 99.6(15) . . ?
C7 N1 Cu1 102.9(15) . . ?
C13 N2 C5 152(3) . . ?
C13 N2 O4 112.8(17) . . ?
C5 N2 O4 40.6(12) . . ?
C13 N2 Cu2 107.2(19) . . ?
C5 N2 Cu2 98.7(14) . . ?
O4 N2 Cu2 139.2(11) . . ?
C1 N3 C19 128.9(15) . . ?
C1 N3 Cu3 116.4(13) . . ?
C19 N3 Cu3 114.2(11) . . ?
C1 O1 Ni1 102.9(14) . . ?
C2 O2 Ni1 105.6(16) . . ?
C2 O3 Cu3 113.5(14) . . ?
C5 O4 N2 39.9(10) . . ?
C5 O4 Ni1 97.6(15) . . ?
N2 O4 Ni1 137.5(12) . . ?
C6 O5 Ni1 101.2(12) . . ?
C6 O6 Cu2 113.5(14) . . ?
C3 O7 Ni1 101.7(13) . . ?
C4 O8 Ni1 110.5(13) . . ?
C4 O9 Cu1 105.2(11) . . ?
O1 C1 N3 105.2(15) . . ?
O1 C1 C2 138(2) . . ?
N3 C1 C2 116.9(18) . . ?
O2 C2 O3 122(2) . . ?
O2 C2 C1 115(2) . . ?
O3 C2 C1 123(2) . . ?
O7 C3 C4 132(2) . . ?
O7 C3 N1 100.0(19) . . ?
C4 C3 N1 128.0(19) . . ?
O8 C4 C3 115.5(17) . . ?
O8 C4 O9 114.6(14) . . ?
C3 C4 O9 129.9(17) . . ?
N2 C5 O4 100(2) . . ?
N2 C5 C6 126(2) . . ?
O4 C5 C6 135(2) . . ?
N2 C5 Ni1 153.1(17) . . ?
O4 C5 Ni1 53.6(12) . . ?
C6 C5 Ni1 80.9(12) . . ?
O6 C6 O5 111.3(15) . . ?
O6 C6 C5 127.6(19) . . ?
O5 C6 C5 121.0(18) . . ?
N1 C7 C10 149.1(13) . . ?
N1 C7 C8 99.5(17) . . ?
C10 C7 C8 107.4(13) . . ?
C9 C8 C7 121.3(18) . . ?
C9 C8 C12 116.8(16) . . ?
C7 C8 C12 122(2) . . ?
C8 C9 C8 124(2) . 10_556 ?
C7 C10 C7 138.8(9) . 10_556 ?
C7 C10 C11 110.6(4) . . ?
C7 C10 C11 110.6(4) 10_556 . ?
N2 C13 C16 144(3) . . ?
N2 C13 C14 120.6(19) . . ?
C16 C13 C14 92(3) . . ?
C15 C14 C13 117.5(16) . . ?
C15 C14 C18 129.2(18) . . ?
C13 C14 C18 113.2(19) . . ?
C14 C15 C14 133(2) 10_557 . ?
C13 C16 C13 168(5) 10_557 . ?
C13 C16 C17 96(2) 10_557 . ?
C13 C16 C17 96(2) . . ?
C22 C19 C20 117.2(14) . . ?
C22 C19 N3 123.5(10) . . ?
C20 C19 N3 119.3(14) . . ?
C21 C20 C19 110.9(15) . . ?
C21 C20 C24 118.4(10) . . ?
C19 C20 C24 130.7(11) . . ?
C20 C21 C20 136.5(19) . 10_557 ?
C19 C22 C19 127.5(16) . 10_557 ?
C19 C22 C23 116.3(8) . . ?
C19 C22 C23 116.3(8) 10_557 . ?
N4L Pd1 N3L 135(3) . . ?
N4L Pd1 O2L 75(3) . . ?
N3L Pd1 O2L 59.5(7) . . ?
N4L Pd1 N1L 108.1(17) . . ?
N3L Pd1 N1L 117(3) . . ?
O2L Pd1 N1L 177(3) . . ?
N5L Pd2 N8L 175.8(9) . . ?
N5L Pd2 N7L 91.8(6) . . ?
N8L Pd2 N7L 92.4(7) . . ?
N5L Pd2 N6L 90.7(6) . . ?
N8L Pd2 N6L 85.1(6) . . ?
N7L Pd2 N6L 177.5(8) . . ?
Pd1 O2L Pd1 152(4) . 15_665 ?
O6W Au1 O6W 90.2(15) . 10_556 ?
O6W Au1 Au1 133.1(8) . 5_656 ?
O6W Au1 Au1 133.1(8) 10_556 5_656 ?
O6W Au1 O8W 79.7(11) . 10_556 ?
O6W Au1 O8W 163.0(13) 10_556 10_556 ?
Au1 Au1 O8W 61.7(7) 5_656 10_556 ?
O6W Au1 O8W 163.0(13) . . ?
O6W Au1 O8W 79.7(11) 10_556 . ?
Au1 Au1 O8W 61.7(7) 5_656 . ?
O8W Au1 O8W 107(2) 10_556 . ?
O6W Au1 O7W 76.2(8) . 10_556 ?
O6W Au1 O7W 138.7(11) 10_556 10_556 ?
Au1 Au1 O7W 59.6(5) 5_656 10_556 ?
O8W Au1 O7W 52.0(15) 10_556 10_556 ?
O8W Au1 O7W 120.3(10) . 10_556 ?
O6W Au1 O7W 138.7(11) . . ?
O6W Au1 O7W 76.2(8) 10_556 . ?
Au1 Au1 O7W 59.6(5) 5_656 . ?
O8W Au1 O7W 120.3(10) 10_556 . ?
O8W Au1 O7W 52.0(15) . . ?
O7W Au1 O7W 88.7(13) 10_556 . ?
S1 Au2 S1 120.9(12) 15_665 . ?
S1 Au2 C1S 44.6(7) 15_665 15_665 ?
S1 Au2 C1S 90.6(14) . 15_665 ?
S1 Au2 C1S 90.6(14) 15_665 . ?
S1 Au2 C1S 44.6(7) . . ?
C1S Au2 C1S 49.1(12) 15_665 . ?
C3S S1 C1S 63(4) . . ?
C3S S1 Au2 136(4) . . ?
C1S S1 Au2 73.3(19) . . ?
O1S C2S C1S 129(4) . . ?
C2S C1S S1 111(3) . . ?
C2S C1S Au2 125(7) . . ?
S1 C1S Au2 62.2(15) . . ?
Au1 O7W Au1 60.8(10) . 5_656 ?
Au1 O8W Au1 56.5(14) 5_656 . ?
 
_refine_diff_density_max    0.896
_refine_diff_density_min   -1.241
_refine_diff_density_rms    0.180

# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000 -0.004      3357      1382 ' '
   2  0.000  0.258  0.500        39        27 ' '
   3  0.000  0.425  0.500         8         4 ' '
   4  0.000  0.575  0.500         8         4 ' '
   5  0.000  0.742  0.500        39        36 ' '
   6  0.105  0.500  0.146         8         6 ' '
   7  0.105  0.500  0.854         8         4 ' '
   8  0.500  0.500  0.465      4230      1391 ' '
   9  0.258  0.000  0.500        39        29 ' '
  10  0.425  0.000  0.500         8         3 ' '
  11  0.500  0.106  0.146         8         5 ' '
  12  0.500  0.106  0.854         8         9 ' '
  13  0.500  0.894  0.146         8         5 ' '
  14  0.500  0.894  0.854         8         8 ' '
  15  0.575  0.000  0.500         8         5 ' '
  16  0.742  0.000  0.500        39        38 ' '
  17  0.894  0.500  0.146         8        10 ' '
  18  0.894  0.500  0.854         8         8 ' '
_platon_squeeze_details
;
;
_shelxl_version_number 2013-4


