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_4334723
_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            'C20 H37 Co N4 O2'
_chemical_formula_weight         424.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   11.0676(8)
_cell_length_b                   11.0757(7)
_cell_length_c                   18.9461(14)
_cell_measurement_temperature    100(2)
_cell_volume                     2322.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            109839
_diffrn_reflns_theta_full        30.62
_diffrn_reflns_theta_max         30.62
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7206
_exptl_absorpt_correction_T_min  0.5558
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.549(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         7166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                6913
_reflns_number_total             7166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400337m_si_002_1.cif
_cod_data_source_block           lk699_p212121_s
_cod_database_code               4334723