Palladium(II) Weak-Link Approach Complexes Bearing Hemilabile N-Heterocyclic Carbene-Thioether Ligands.
Liu, Yuan; Kean, Zachary S.; d'Aquino, Andrea I; Manraj, Yashin D.; Mendez-Arroyo, Jose; Mirkin, Chad A.; Inorganic chemistry 56 (2017) 5902–5910; doi:10.1021/acs.inorgchem.7b00543

data_4345853
_publ_section_title
;
 Palladium(II) Weak-Link Approach Complexes Bearing Hemilabile
 N-Heterocyclic Carbene-Thioether Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5902
_journal_page_last               5910
_journal_paper_doi               10.1021/acs.inorgchem.7b00543
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C30 H40 N4 Pd S2, 2(B F4)'
_chemical_formula_sum            'C30 H40 B2 F8 N4 Pd S2'
_chemical_formula_weight         800.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.499(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.558(8)
_cell_length_b                   12.607(8)
_cell_length_c                   22.224(14)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.569
_cell_measurement_theta_min      2.489
_cell_volume                     3421(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            102619
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.553
_diffrn_reflns_theta_min         2.355
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0770 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.9377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+1.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9016
_reflns_number_total             10386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00543_si_003.cif
_cod_data_source_block           cx0782
_cod_depositor_comments          'Adding full bibliography for 4345853.cif.'
_cod_database_code               4345853
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.769
_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:
 C7(H7A,H7B), C8(H8A,H8B), C22(H22A,H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              70411
_shelx_hkl_checksum              21055
_olex2_date_sample_data_collection 2016-06-06
_olex2_date_sample_submission    2016-06-02
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in Paratone oil'
_olex2_submission_original_sample_id cx0782
_olex2_submission_special_instructions 'No special instructions were received'