Difference in Energy between Two Distinct Types of Chalcogen Bonds Drives Regioisomerization of Binuclear (Diaminocarbene)Pd<sup>II</sup> Complexes.
Mikherdov, Alexander S.; Kinzhalov, Mikhail A.; Novikov, Alexander S.; Boyarskiy, Vadim P.; Boyarskaya, Irina A.; Dar'in, Dmitry V.; Starova, Galina L.; Kukushkin, Vadim Yu; Journal of the American Chemical Society 138 (2016) 14129–14137; doi:10.1021/jacs.6b09133

data_4131062
_publ_section_title
;
 Difference in Energy between Two Distinct Types of Chalcogen Bonds Drives
 Regioisomerization of Binuclear (Diaminocarbene)Pd<sup>II</sup>
 Complexes.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14129
_journal_page_last               14137
_journal_paper_doi               10.1021/jacs.6b09133
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C39 H38 Cl2 N6 Pd2 S'
_chemical_formula_sum            'C39 H38 Cl2 N6 Pd2 S'
_chemical_formula_weight         906.51
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-20
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                86.541(3)
_cell_angle_beta                 88.545(2)
_cell_angle_gamma                85.128(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5879(2)
_cell_length_b                   8.2580(3)
_cell_length_c                   30.4025(9)
_cell_measurement_reflns_used    6373
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9230
_cell_measurement_theta_min      4.3660
_cell_volume                     1894.31(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9529
_diffrn_measured_fraction_theta_max 0.9529
_diffrn_measurement_details
;
  1 omega -113.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000 -180.0000 99

  2 omega  -30.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000   60.0000 65

  3 omega -119.00  -20.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -19.0000  -90.0000 99

  4 omega    8.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -90.0000 27

  5 omega   85.00  130.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000   90.0000 45

  6 omega   92.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000  -60.0000 29

  7 omega   58.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787 -178.0000 -150.0000 56

  8 omega   52.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 39

  9 omega   29.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   90.0000 60

 10 omega   68.00  100.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   19.0000   68.0333 32

 11 omega   62.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 40

 12 omega   59.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 27

 13 omega   53.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 25

 14 omega   57.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 41

 15 omega  136.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  150.0000 42

 16 omega   71.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -60.0000 27

 17 omega   38.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -30.0000 59

 18 omega   91.00  139.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 48

 19 omega  114.00  140.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 26

 20 omega  144.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 33

 21 omega   41.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 35

 22 omega   66.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   60.0000 48

 23 omega   46.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 31

 24 omega  107.00  132.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 25

 25 omega   52.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -90.0000 43

 26 omega   33.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -30.0000 74

 27 omega   33.00   94.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 61

 28 omega  140.00  174.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 34

 29 omega   62.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 46

 30 omega   67.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   60.0000 36

 31 omega   85.00  110.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 25

 32 omega  111.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   60.0000 65

 33 omega   53.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   60.0000 25

 34 omega   45.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 31

 35 omega   56.00   81.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0309589000
_diffrn_orient_matrix_UB_12      0.0135437000
_diffrn_orient_matrix_UB_13      0.0494796000
_diffrn_orient_matrix_UB_21      -0.0697245000
_diffrn_orient_matrix_UB_22      0.1808996000
_diffrn_orient_matrix_UB_23      -0.0039668000
_diffrn_orient_matrix_UB_31      -0.1889909000
_diffrn_orient_matrix_UB_32      -0.0476181000
_diffrn_orient_matrix_UB_33      0.0106846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            16320
_diffrn_reflns_theta_full        72.48
_diffrn_reflns_theta_max         72.48
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tables
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.368
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0601
_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/[\s^2^(Fo^2^)+(0.0386P)^2^+25.9736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                6131
_reflns_number_total             7256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b09133_si_002.cif
_cod_data_source_block           kr1
_cod_original_cell_volume        1894.30(11)
_cod_database_code               4131062
_chemical_oxdiff_formula         'pd2 cl2 c39 h38 n6 s1'
_reflns_odcompleteness_completeness 90.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95