Homogeneous Nickel Catalysts for the Selective Transfer of a Single Arylthio Group in the Catalytic Hydrothiolation of Alkynes
Malyshev, Denis A.; Scott, Natalie M.; Marion, Nicolas; Stevens, Edwin D.; Ananikov, Valentine P.; Beletskaya, Irina P.; Nolan, Steven P.; Organometallics 25 (2006) 4462–; doi:10.1021/om060302v

data_4075464
_publ_section_title
;
 Homogeneous Nickel Catalysts for the Selective Transfer of a Single
 Arylthio Group in the Catalytic Hydrothiolation of Alkynes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4462
_journal_paper_doi               10.1021/om060302v
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C38 H46 N2 Ni S'
_chemical_formula_weight         621.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.7840(10)
_cell_angle_beta                 78.4200(10)
_cell_angle_gamma                66.0720(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2460(3)
_cell_length_b                   9.3525(3)
_cell_length_c                   21.5658(8)
_cell_measurement_reflns_used    19280
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.574
_cell_measurement_theta_min      2.385
_cell_volume                     1667.99(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19087
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.910052
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0001(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         11651
_refine_ls_number_restraints     791
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.722
_refine_ls_shift/su_mean         0.137
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.2378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                10159
_reflns_number_total             11651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060302vsi20060405_105716.cif
_cod_data_source_block           nol311m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4075464