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_4131065
_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, C4 H10 O'
_chemical_formula_sum            'C43 H48 Cl2 N6 O Pd2 S'
_chemical_formula_weight         980.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-19
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7589(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.07769(12)
_cell_length_b                   19.4303(3)
_cell_length_c                   27.7228(5)
_cell_measurement_reflns_used    17502
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4348
_cell_measurement_theta_min      3.1859
_cell_volume                     4350.77(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_details
;
  1 omega  -86.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1287  126.0000   30.0000 68

  2 omega  -50.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1287   38.0000  150.0000 80

  3 omega -136.00 -103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -112.0000   60.0000 33

  4 omega -118.00  -92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -112.0000 -120.0000 26

  5 omega   71.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   60.0000 25

  6 omega   80.00  106.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  153.0000  -90.0000 26

  7 omega  145.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  -30.0000 33

  8 omega   87.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 26

  9 omega   35.00   76.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 41

 10 omega   52.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 46

 11 omega   65.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   90.0000 29

 12 omega   44.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 46

 13 omega   31.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -150.0000 73

 14 omega  122.00  156.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -150.0000 34

 15 omega   55.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -30.0000 26

 16 omega   84.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -60.0000 39

 17 omega   88.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -30.0000 28

 18 omega   40.00   65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 25

 19 omega  124.00  167.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  153.0000  -90.0000 43

 20 omega  101.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  -30.0000 29

 21 omega   35.00   60.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 25

 22 omega -114.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1287  -57.0000    0.0000 97

 23 omega  -83.00  -58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1287 -153.0000   90.0000 25

 24 omega  -49.00   17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1287   38.0000  -60.0000 66

 25 omega   12.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1287   57.0000 -120.0000 99

 26 omega  -40.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000 -150.0000 29

 27 omega -100.00  -61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -45.0000   30.0000 39

 28 omega   31.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 49

 29 omega  114.00  159.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   -5.0000   77.0782 45

 30 omega   86.00  112.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -82.0000  146.1539 26

 31 omega   47.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   90.0000 25

 32 omega   84.00  162.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 78

 33 omega   54.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -90.0000 26

 34 omega   37.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 29

 35 omega  150.00  161.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  150.0000 11
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1132305000
_diffrn_orient_matrix_UB_12      0.0571959000
_diffrn_orient_matrix_UB_13      0.0204415000
_diffrn_orient_matrix_UB_21      0.0263416000
_diffrn_orient_matrix_UB_22      0.0277336000
_diffrn_orient_matrix_UB_23      -0.0514160000
_diffrn_orient_matrix_UB_31      -0.1512293000
_diffrn_orient_matrix_UB_32      0.0473455000
_diffrn_orient_matrix_UB_33      0.0053693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34999
_diffrn_reflns_theta_full        76.63
_diffrn_reflns_theta_max         76.63
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.366
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0391
_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/[\s^2^(Fo^2^)+(0.0583P)^2^+8.7398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                7942
_reflns_number_total             8963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b09133_si_002.cif
_cod_data_source_block           tr1
_cod_database_code               4131065
_chemical_oxdiff_formula         'c20 h18 br1 pt1'
_reflns_odcompleteness_completeness 93.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95