Experimental and Computational Investigation of Thiolate Alkylation in NiII and ZnII Complexes: Role of the Metal on the Sulfur Nucleophilicity
Marcello Gennari; Marius Retegan; Serena DeBeer; Jacques Pécaut; Frank Neese; Marie-Noëlle Collomb; Carole Duboc; Inorganic Chemistry 50 (2011) 10047–10055; doi:10.1021/ic200899w

data_4326460
_publ_section_title
;
 Experimental and Computational Investigation of Thiolate Alkylation in
 NiII and ZnII Complexes: Role of the Metal on the Sulfur Nucleophilicity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10047
_journal_page_last               10055
_journal_paper_doi               10.1021/ic200899w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H36 I2 N2 S2 Zn'
_chemical_formula_weight         928.00
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 94.874(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5525(6)
_cell_length_b                   32.172(2)
_cell_length_c                   15.6826(12)
_cell_measurement_reflns_used    2299
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_cell_measurement_theta_max      32.5079
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega   39.00   98.00   1.0000  360.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -90.0000 59

  2 omega   36.00   78.00   1.0000  360.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000 -150.0000 42

  3 omega   32.00   98.00   1.0000  360.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000 -150.0000 66

  4 omega  -95.00   -1.00   1.0000  360.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -37.0000  -90.0000 94

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.1568
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12794
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    2.413
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.7303
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.629
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.629
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0364
_reflns_number_gt                2447
_reflns_number_total             5315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200899w_si_003.cif
_cod_data_source_block           znl''i2
_cod_original_cell_volume        3796.7(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4326460