Synthesis, Characterization, and Electrochemical Properties of a Series of Sterically Varied Iron(II) Alkoxide Precursors and Their Resultant Nanoparticles
Timothy J. Boyle; Leigh Anna M. Ottley; Christopher A. Apblett; Constantine A. Stewart; Sarah M. Hoppe; Krista L. Hawthorne; Mark A. Rodriguez; Inorganic Chemistry 50 (2011) 6174–6182; doi:10.1021/ic200423m

data_4325490
_publ_section_title
;
 Synthesis, Characterization, and Electrochemical Properties of a Series
 of Sterically Varied Iron(II) Alkoxide Precursors and Their Resultant
 Nanoparticles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6174
_journal_page_last               6182
_journal_paper_doi               10.1021/ic200423m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C31 H33 Fe N3 O2'
_chemical_formula_weight         535.45
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 104.329(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5680(19)
_cell_length_b                   11.6850(16)
_cell_length_c                   19.236(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2954.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8802
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.111
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0411P)^2^+1.6925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1895
_reflns_number_total             2125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200423m_si_001_04.cif
_cod_data_source_block           9nv241s
_cod_database_code               4325490