N-Arylcyano-β-diketiminate Methallyl Nickel Complexes: Synthesis, Adduct Formation, and Reactivity toward Ethylene
Trofymchuk, Oleksandra S.; Gutsulyak, Dmitry V.; Quintero, Celso; Parvez, Masood; Daniliuc, Constantin G.; Piers, Warren E.; Rojas, Rene S.; Organometallics 32 (2013) 7323–; doi:10.1021/om400847b

data_4082102
_publ_section_title
;
 N-Arylcyano-\b-diketiminate Methallyl Nickel Complexes: Synthesis, Adduct
 Formation, and Reactivity toward Ethylene
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7323
_journal_paper_doi               10.1021/om400847b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C19 H16 N4'
_chemical_formula_weight         300.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'at N1 form difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.509(2)
_cell_angle_beta                 96.671(2)
_cell_angle_gamma                104.723(2)
_cell_formula_units_Z            4
_cell_length_a                   9.2851(3)
_cell_length_b                   9.5028(3)
_cell_length_c                   19.0924(6)
_cell_measurement_reflns_used    3598
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      4.08
_cell_volume                     1611.03(9)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '&#x00DF;w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7755
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.7674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                3989
_reflns_number_total             5474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400847b_si_002.cif
_cod_data_source_block           erk5925
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082102