Structure and Dynamics of Neutral β-H Agostic Nickel Alkyls: A Combined Experimental and Theoretical Study
Elzbieta Kogut; Alexander Zeller; Timothy H. Warren; Thomas Strassner; Journal of the American Chemical Society 126 (2004) 11984–11994; doi:10.1021/ja0477221

data_4112970
_publ_contact_author             'Timothy H. Warren'
_publ_contact_author_email       thw@georgetown.edu
_publ_section_title
;
 Structure and Dynamics of Neutral \b-H Agostic Nickel Alkyls: A Combined
 Experimental and Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11984
_journal_page_last               11994
_journal_paper_doi               10.1021/ja0477221
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C23 H30 N2 Ni'
_chemical_formula_weight         393.20
_chemical_name_common            {Me2NN]Ni(CH2CH3)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.51(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.113(8)
_cell_length_b                   8.758(7)
_cell_length_c                   19.98(2)
_cell_measurement_reflns_used    4087
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.784
_cell_measurement_theta_min      2.627
_cell_volume                     2101(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics
'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23090
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       chunck
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5042
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                3069
_reflns_number_total             5042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0477221si20040729_092119.cif
_cod_data_source_block           c:\papers\final-~1\cmpd_3\sad
_cod_database_code               4112970