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_4131064
_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         '2(C44 H41 Cl2 N7 Pd2 S), 0.5(C4 O2)'
_chemical_formula_sum            'C90 H82 Cl4 N14 O Pd4 S2'
_chemical_formula_weight         2007.22
_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             2015-10-16
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.916(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7979(6)
_cell_length_b                   20.6001(10)
_cell_length_c                   15.3163(7)
_cell_measurement_reflns_used    10291
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1220
_cell_measurement_theta_min      3.1140
_cell_volume                     4343.3(3)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_details
;
  1 omega  -25.00   14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -99.0000 -120.0000 39

  2 omega  -87.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -57.0000   60.0000 72

  3 omega  -25.00    0.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -99.0000  -30.0000 25

  4 omega  -86.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -19.0000   90.0000 112

  5 omega   20.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339   77.0000 -120.0000 28

  6 omega  -77.00  -50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339 -178.0000 -120.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0271459000
_diffrn_orient_matrix_UB_12      0.0113071000
_diffrn_orient_matrix_UB_13      -0.0379465000
_diffrn_orient_matrix_UB_21      0.0436177000
_diffrn_orient_matrix_UB_22      0.0042308000
_diffrn_orient_matrix_UB_23      -0.0213536000
_diffrn_orient_matrix_UB_31      -0.0037418000
_diffrn_orient_matrix_UB_32      -0.0322569000
_diffrn_orient_matrix_UB_33      -0.0160700000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26140
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.67
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79127
_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            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.119
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+10.9735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                8482
_reflns_number_total             9729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b09133_si_002.cif
_cod_data_source_block           kr9
_cod_database_code               4131064
_chemical_oxdiff_formula         'c40 h38 n4 s1 pd1 cl2'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32