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_4131066
_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         'C38 H37 Cl2 N7 Pd2 S, C H Cl3'
_chemical_formula_sum            'C39 H38 Cl5 N7 Pd2 S'
_chemical_formula_weight         1026.87
_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     iterative
_audit_creation_date             2016-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.573(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1558(3)
_cell_length_b                   18.5007(9)
_cell_length_c                   27.9197(11)
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2714
_cell_measurement_theta_min      2.6387
_cell_volume                     4199.3(3)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -95.00  -34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  178.0000   60.0000 61

  2 omega  -24.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -99.0000   60.0000 48

  3 omega  -14.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339   38.0000   60.0000 66

  4 omega  -40.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -19.0000   60.0000 64

  5 omega  -88.00  -27.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -77.0000 -180.0000 61

  6 omega  -25.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0339  -99.0000 -120.0000 49

  7 omega  -11.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714   77.0000   30.0000 100

  8 omega  -51.00  -26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -77.0000  -60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0040839000
_diffrn_orient_matrix_UB_12      -0.0055357000
_diffrn_orient_matrix_UB_13      0.0251990000
_diffrn_orient_matrix_UB_21      -0.0180099000
_diffrn_orient_matrix_UB_22      0.0370817000
_diffrn_orient_matrix_UB_23      0.0034021000
_diffrn_orient_matrix_UB_31      -0.0852551000
_diffrn_orient_matrix_UB_32      -0.0081110000
_diffrn_orient_matrix_UB_33      -0.0016394000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            39391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75176
_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    1.624
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+7.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7931
_reflns_number_total             9549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09133_si_002.cif
_cod_data_source_block           tr7
_cod_database_code               4131066
_chemical_oxdiff_formula         'C26 H17 cl2 n8 pd2 s1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C18(H18), C34(H34), C11(H11), C26(H26), C35(H35), C33(H33),
 C19(H19), C17(H17), C2(H2), C9(H9), C10(H10), C25(H25)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C29(H29A,H29B,
 H29C), C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'