Unsymmetrical Chelation of N-Thioether-Functionalized Bis(diphenylphosphino)amine-Type Ligands and Substituent Effects on the Nuclearity of Iron(II) Complexes: Structures, Magnetism, and Bonding.
Fliedel, Christophe; Rosa, Vitor; Falceto, Andrés; Rosa, Patrick; Alvarez, Santiago; Braunstein, Pierre; Inorganic chemistry 54 (2015) 6547–6559; doi:10.1021/acs.inorgchem.5b00834

data_4343423
_publ_section_title
;
 Unsymmetrical Chelation of N-Thioether-Functionalized
 Bis(diphenylphosphino)amine-Type Ligands and Substituent Effects on the
 Nuclearity of Iron(II) Complexes: Structures, Magnetism, and Bonding.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6547
_journal_page_last               6559
_journal_paper_doi               10.1021/acs.inorgchem.5b00834
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C64 H57 Fe N2 O2 P4 S2, F6 P'
_chemical_formula_sum            'C64 H57 F6 Fe N2 O2 P5 S2'
_chemical_formula_weight         1274.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.899(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7306(2)
_cell_length_b                   25.6029(8)
_cell_length_c                   23.5000(6)
_cell_measurement_reflns_used    27861
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6177.5(3)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1510
_diffrn_reflns_av_unetI/netI     0.1599
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35353
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.205
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 The residual electron density was assigned to a molecule of the 
 pentane solvent [203/4 = 51 e per asymmetric unit; one molecule
 of C5H12 would give 42e].
;
_refine_diff_density_max         0.747
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         14119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8319
_reflns_number_total             14119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00834_si_002.cif
_cod_data_source_block           vitor26
_cod_depositor_comments
'Adding full bibliography for 4343421--4343423.cif.'
_cod_database_code               4343423
_shelxl_version_number           2013-4
_shelx_res_checksum              58785
_shelx_hkl_checksum              25591