Synthesis of Monomeric Fe(II) and Ru(II) Complexes of Tetradentate Phosphines
Barun Jana; Arkady Ellern; Oleg Pestovsky; Aaron Sadow; Andreja Bakac; Inorganic Chemistry 50 (2011) 3010–3016; doi:10.1021/ic102510c

data_4324780
_publ_contact_author_address
;1605 Gilman Hall
Department of Chemistry
Iowa State University
Ames IA 50011
;
_publ_contact_author_email       sadow@iastate.edu
_publ_contact_author_fax         +1-515-294-0105
_publ_contact_author_name        'Aaron D. Sadow'
_publ_contact_author_phone       +1-515-294-8069
_publ_section_title
;
 Synthesis of Monomeric Fe(II) and Ru(II) Complexes of Tetradentate
 Phosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3010
_journal_page_last               3016
_journal_paper_doi               10.1021/ic102510c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C53 H52 F6 Fe N2 O8 P4 S2'
_chemical_formula_weight         1202.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 116.6550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.1508(8)
_cell_length_b                   21.6884(8)
_cell_length_c                   23.7433(8)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.21
_cell_volume                     11114.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            112802
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.9097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         27185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+8.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                17748
_reflns_number_total             27185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102510c_si_002_5.cif
_cod_data_source_block           '[P4Fe(NCMe)2]OTf2'
_cod_database_code               4324780