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_4131067
_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 H39 Cl2 N7 Pd2 S, C H2 Cl2'
_chemical_formula_sum            'C40 H41 Cl4 N7 Pd2 S'
_chemical_formula_weight         1006.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.09548(14)
_cell_length_b                   19.5379(3)
_cell_length_c                   27.0319(4)
_cell_measurement_reflns_used    22431
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.8890
_cell_measurement_theta_min      3.0140
_cell_volume                     4275.60(12)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -7.00   43.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -      -25.2468   57.0000   30.0000 50

  2 omega  -81.00  -37.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -      -25.2468  -38.0000    0.0000 44

  3 omega  -99.00  -35.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -      -25.2468 -178.0000  120.0000 64

  4 omega    5.00   95.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -       26.3406   57.0000  -90.0000 90

  5 omega  -42.00   44.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -       26.3406  -57.0000  120.0000 86

  6 omega    0.00   50.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -       26.3406  -77.0000 -120.0000 50

  7 omega    1.00   99.00   1.0000   35.4100
omega____ theta____ kappa____ phi______ frames
    -       26.3406   38.0000   30.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0291069000
_diffrn_orient_matrix_UB_12      -0.0222745000
_diffrn_orient_matrix_UB_13      0.0187965000
_diffrn_orient_matrix_UB_21      -0.0180684000
_diffrn_orient_matrix_UB_22      -0.0252117000
_diffrn_orient_matrix_UB_23      -0.0180868000
_diffrn_orient_matrix_UB_31      0.0806429000
_diffrn_orient_matrix_UB_32      -0.0136894000
_diffrn_orient_matrix_UB_33      0.0027259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            41352
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.626
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 4061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+5.1746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9506
_reflns_number_total             9844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09133_si_002.cif
_cod_data_source_block           tr8
_cod_database_code               4131067
_chemical_oxdiff_formula         'Pd C18 Cl2 N2 H18'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C18(H18), C19(H19), C20(H20), C26(H26), C27(H27),
 C11(H11), C28(H28), C34(H34), C36(H36), C35(H35)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C31(H31A,H31B,
 H31C), C30(H30A,H30B,H30C), C15(H15A,H15B,H15C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              15197
_shelx_hkl_checksum              10325
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 1444230786.04
_olex2_submission_special_instructions 'No special instructions were received'