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_4325488
_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            'C33 H37 Fe N3 O2'
_chemical_formula_weight         563.51
_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                 110.544(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   34.823(4)
_cell_length_b                   16.292(2)
_cell_length_c                   17.320(2)
_cell_measurement_temperature    173(2)
_cell_volume                     9201.3(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27940
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            maroon
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                4858
_reflns_number_total             6619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200423m_si_001_02.cif
_cod_data_source_block           9fb172s
_cod_original_cell_volume        9201(2)
_cod_database_code               4325488