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_4324777
_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            'C41 H40 Br2 Fe P4'
_chemical_formula_weight         872.28
_chemical_name_common            'Sad170, Barun Jana, Sadow'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.3-0'
_cell_angle_alpha                90
_cell_angle_beta                 99.510(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4019(11)
_cell_length_b                   34.565(4)
_cell_length_c                   22.463(3)
_cell_measurement_reflns_used    1370
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      19.7602
_cell_measurement_theta_min      2.2365
_cell_volume                     7199.6(15)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  ' BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12881
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    2.848
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12881
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+6.5903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                8918
_reflns_number_total             12881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102510c_si_002_2.cif
_cod_data_source_block           P4FeBr2
_cod_original_cell_volume        7199.6(14)
_cod_database_code               4324777