Mesoionic Triazolylidene Nickel Complexes: Synthesis, Ligand Lability, and Catalytic C‒C Bond Formation Activity
Wei, Yingfei; Petronilho, Ana; Mueller-Bunz, Helge; Albrecht, Martin; Organometallics 33 (2014) 5834–; doi:10.1021/om500593s

data_4084104
_publ_section_title
;
 Mesoionic Triazolylidene Nickel Complexes: Synthesis, Ligand Lability,
 and Catalytic C--C Bond Formation Activity
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5834
_journal_paper_doi               10.1021/om500593s
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H39 N6 Ni, I, 0.469 (C7 H8)'
_chemical_formula_sum            'C34.283 H42.752 I N6 Ni'
_chemical_formula_weight         724.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2509(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.80156(5)
_cell_length_b                   19.60167(7)
_cell_length_c                   15.81324(6)
_cell_measurement_reflns_used    44451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7380
_cell_measurement_theta_min      3.5910
_cell_volume                     3321.34(2)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69666
_diffrn_reflns_theta_full        76.88
_diffrn_reflns_theta_max         76.88
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    8.383
_exptl_absorpt_correction_T_max  0.409
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1485.8
_exptl_crystal_size_max          0.2833
_exptl_crystal_size_mid          0.2112
_exptl_crystal_size_min          0.1533
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(2)
_refine_ls_extinction_coef       0.00065(3)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         13915
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+3.0024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                13523
_reflns_number_total             13915
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om500593s_si_002.cif
_cod_data_source_block           alb268(4aI)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4084104