The self-assembly of a cyclometalated palladium photosensitizer into proteins-stabilized nanorods triggered drug uptake in vitro and in vivo.
Zhou, Xue-Quan; Xiao, Ming; Vadde, Ramu; Hilgendorf, Jonathan; Li, Xuezhao; Papadopoulou, Panagiota; Siegler, Maxime A.; Kros, Alexander; Sun, Wen; Bonnet, Sylvestre; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01369

data_4135031
_publ_section_title
;
 The self-assembly of a cyclometalated palladium photosensitizer into
 proteins-stabilized nanorods triggered drug uptake in vitro and in vivo.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01369
_journal_year                    2020
_chemical_formula_moiety         'C22 H17 N4 Pd, F6 P'
_chemical_formula_sum            'C22 H17 F6 N4 P Pd'
_chemical_formula_weight         588.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                111.199(3)
_cell_angle_beta                 98.922(3)
_cell_angle_gamma                94.144(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0794(2)
_cell_length_b                   12.4486(4)
_cell_length_c                   12.4689(4)
_cell_measurement_reflns_used    7723
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      6.36
_cell_volume                     1002.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12084
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.845
_diffrn_reflns_theta_min         3.846
_exptl_absorpt_coefficient_mu    8.930
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3974
_reflns_number_total             4342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01369_si_003.cif
_cod_data_source_block           2_PF6
_cod_database_code               4135031
_shelx_shelxl_version_number     2018/3
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 2 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (   7.077   12.448   12.462   111.22    98.89    94.15)
Matrix 2 is taken from component 2 (   7.073   12.460   12.437   111.26    98.26    94.57)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   1.0004  -0.0002  -0.0005    -0.2680  -0.9996  -0.0003    -0.5260  -0.0002  -1.0003   det 1.000653
TL-1=UB[2]*UB[1]-1:   0.9993  -0.0002  -0.0005    -0.2677  -1.0003   0.0004    -0.5254   0.0003  -0.9995   det 0.999348
Rot= 179.9827 deg around the following vectors: 
Reciprocal space (hkl): 0.9591 -0.1285 -0.2523
Direct space (uvw)    : 1.0000 -0.0012 0.0025
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 2 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN INFO: Face list of component 1 
  1:   0.3454   2.5188  -8.0471  d=   0.0141
  2:  -0.0776  -4.8609  -4.0418  d=   0.0207
  3:   4.5627   0.1502  -2.0533  d=   0.0757
  4:   0.0776   4.8609   4.0418  d=   0.0155
  5:  -4.3525  -1.6165   0.7225  d=   0.0590
  6:  -0.0024  -5.0015   7.9962  d=   0.0151
  7:   0.9961  -6.9948  -1.9952  d=   0.0405
  8:  -0.0019  -4.0023   7.9958  d=   0.0125
  9:   3.9968  -1.0041   1.0040  d=   0.0714
 10:   0.0024   5.0015  -7.9962  d=   0.0135
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:   0.3483  -2.6151   7.8621  d=   0.0141
  2:  -0.0746   4.8816   4.0788  d=   0.0207
  3:   4.5604  -1.3726  -0.3451  d=   0.0757
  4:   0.0746  -4.8816  -4.0788  d=   0.0155
  5:  -4.3494   2.7826   1.5643  d=   0.0590
  6:  -0.0049   5.0067  -7.9921  d=   0.0151
  7:   0.9980   6.7294   1.4685  d=   0.0405
  8:  -0.0047   4.0070  -7.9917  d=   0.0125
  9:   3.9937  -0.0653  -3.1038  d=   0.0714
 10:   0.0049  -5.0067   7.9921  d=   0.0135
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 13120 observations read
Component 2: 13141 observations read

23995 composite observations collected (21796 fully isolated, 2199 overlapped), 58 skipped due to one or more missing parts

OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |        872 |     3.6 <--- ALMOST SEPARATED
   0.20 - 0.40  |         72 |     0.3
   0.40 - 0.60  |          3 |     0.0
   0.60 - 0.80  |         21 |     0.1
   0.80 - 1.00  |       1231 |     5.1 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |       2199 |     9.2

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 87.90% (6829 common observations, 2077 merged)
Twin 2: 12.10% (5823 common observations, 2077 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

11830 of 13087 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-619174.0625 max=4319006.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=380.6988 max=15293.3662

SCALING COMPONENT 2

11851 of 13107 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-835853.4375 max=4319006.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=312.3031 max=15293.3662

Computed twin ratios:
Twin 1: 87.98% (6829 common observations, 2077 merged)
Twin 2: 12.02% (5823 common observations, 2077 merged)

DC PROFFITRRPTWIN INFO: Determining HKLF4 overlap threshold for completeness requirement (>=80.0%)
DC PROFFITRRPTWIN INFO: HKLF4 overlap threshold kept - 0.40

DC PROFFITRRPTWIN INFO: Step 6 - Decomposed intensities statistics (HKLF4)
 
COMPONENT 1

 
Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only!
	Mean F2 and F2/sig(F2) are given for all measured values!
Note: The RsigmaA values are computed for all measured values!

Help: For more information about computations of rint and rsigma please look into Crysalis help: 
 file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html
 

Statistics vs intensity - point group symmetry: P-1
                       #        #        #      average    mean      mean        
          intensity measured   kept    unique  redundancy   F2     F2/sig(F2)   Rint   Rsigma
---------------------------------------------------------------------------------------------
   4286979-   176534     1208     1208      358    3.4    333844.08    60.94    0.015    0.016
    176037-   106046     1248     1248      358    3.5    135033.71    41.83    0.019    0.021
    105996-    75881     1255     1255      358    3.5     89502.66    36.45    0.024    0.026
     75845-    54789     1169     1169      358    3.3     64756.02    31.37    0.027    0.029
     54768-    39257     1169     1169      358    3.3     46429.85    27.00    0.030    0.033
     39183-    26533     1183     1183      358    3.3     32650.20    21.21    0.037    0.039
     26522-    16018     1109     1109      358    3.1     21075.45    15.79    0.044    0.046
     16015-     7911     1158     1158      358    3.2     11984.56     9.93    0.065    0.067
      7894-     2548     1149     1149      358    3.2      4940.42     4.67    0.111    0.115
      2539-    -4884     1182     1182      367    3.2      1033.14     1.06    0.383    0.428
-------------------------------------------------------------------------------------------
   4286979-    -4884    11830    11830     3589    3.3     75814.16    25.40    0.023    0.024
 

Statistics vs resolution - point group symmetry: P-1
resolu-      #        #        #               average    mean      mean          
tion(A)   measured   kept    unique           redundancy   F2     F2/sig(F2)   Rint   Rsigma   RsigmaA
------------------------------------------------------------------------------------------------------
 inf-1.68     1171     1171      358             3.3    214006.93    41.86    0.015    0.016     0.018
1.68-1.36      881      881      358             2.5    117392.24    21.71    0.024    0.025     0.035
1.36-1.19     1769     1769      358             4.9     85529.07    24.26    0.028    0.032     0.034
1.19-1.09     1495     1495      358             4.2     63432.14    22.72    0.026    0.028     0.035
1.09-1.01     1286     1286      358             3.6     62073.63    24.47    0.021    0.023     0.033
1.01-0.96     1216     1216      358             3.4     53189.79    23.63    0.021    0.024     0.035
0.96-0.91     1154     1154      358             3.2     48060.02    23.41    0.027    0.029     0.035
0.91-0.87     1082     1082      358             3.0     36424.26    22.15    0.026    0.028     0.038
0.87-0.84      957      957      358             2.7     34051.40    23.97    0.029    0.031     0.035
0.84-0.81      819      819      367             2.2     30231.86    26.09    0.029    0.031     0.032
------------------------------------------------------------------------------------------------------
 inf-0.81    11830    11830     3589             3.3     75814.16    25.40    0.023    0.024     0.030
 

Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1
resolu-      #        #        #       %       average    mean      mean          
tion(A)    kept     theory   unique complete  redundancy   F2     F2/sig(F2)   Rint  RsigmaB
--------------------------------------------------------------------------------------------
 inf-1.68     1171      438      358   81.7      3.3    214006.93    76.80    0.015    0.010
1.68-1.36      881      400      358   89.5      2.5    117392.24    35.26    0.024    0.022
1.36-1.19     1769      395      358   90.6      4.9     85529.07    49.61    0.028    0.017
1.19-1.09     1495      387      358   92.5      4.2     63432.14    45.29    0.026    0.017
1.09-1.01     1286      387      358   92.5      3.6     62073.63    48.08    0.021    0.018
1.01-0.96     1216      381      358   94.0      3.4     53189.79    44.95    0.021    0.019
0.96-0.91     1154      386      358   92.7      3.2     48060.02    44.21    0.027    0.020
0.91-0.87     1082      384      358   93.2      3.0     36424.26    40.55    0.026    0.022
0.87-0.84      957      380      358   94.2      2.7     34051.40    41.37    0.029    0.022
0.84-0.81      819      405      367   90.6      2.2     30231.86    41.38    0.029    0.021
--------------------------------------------------------------------------------------------
 inf-0.81    11830     3944     3589   91.0      3.3     75814.16    47.45    0.023    0.017
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=13087, from those 11830 with overlapping factor < 0.400 written to file D:\Data\xs1926a\twin_abs_twin1_hklf4.hkl, 1257 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2          13087     12084      4358     2.77     25.85     0.017     0.031

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2           2199      1882       876     2.15     28.07     0.021     0.032

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       10888     10202      3482     2.93     25.22     0.017     0.031
     2           0         0         0     0.00      0.00     0.000     0.000

4358 merged reflections saved into file: D:\Data\xs1926a\twin_abs_twin1_hklf5.hkl

Use this hkl file in SHELXL with BASF instruction, which has (components minus 1) entries, and HKLF 5 instruction.
E.g. Two component twin: 'BASF n2' in .ins file, BASF n1 can be computed as n1 = 1.0 - n2.
E.g. Three component twin: 'BASF n2 n3' in .ins file, BASF n1 can be computed as n1 = 1.0 - (n2 + n3).

BASF 0.12024 
;
_oxdiff_exptl_absorpt_empirical_full_min 0.773
_oxdiff_exptl_absorpt_empirical_full_max 1.438
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              37884
_shelx_hkl_checksum              6539