Synthesis, Structure, and Solution Reduction Reactions of Volatile and Thermally Stable Mid to Late First Row Transition Metal Complexes Containing Hydrazonate Ligands
Lakmal C. Kalutarage; Philip D. Martin; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 52 (2013) 5385–5394; doi:10.1021/ic400337m

data_4334726
_publ_section_title
;
 Synthesis, Structure, and Solution Reduction Reactions of Volatile and
 Thermally Stable Mid to Late First Row Transition Metal Complexes
 Containing Hydrazonate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5385
_journal_page_last               5394
_journal_paper_doi               10.1021/ic400337m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C24 H51 N6 Ni1.5 O3'
_chemical_formula_weight         559.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.3403(7)
_cell_length_b                   8.0896(2)
_cell_length_c                   11.1323(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2822.38(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18258
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.046
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_F_000             1212
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.085(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.487
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.487
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+4.7789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                7227
_reflns_number_total             7555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400337m_si_002_4.cif
_cod_data_source_block           lk772_p7a_p21212_s
_cod_original_formula_sum        'C24 H51 N6 Ni1.50 O3'
_cod_database_code               4334726