A New Spin on Cyclooctatetraene (COT) Redox Activity: Low-Spin Iron(I) Complexes That Exhibit Antiferromagnetic Coupling to a Singly Reduced η4-COT Ligand
Mukhopadhyay, Tufan K.; Flores, Marco; Feller, Russell K.; Scott, Brian L.; Taylor, R. Dean; Paz-Pasternak, Moshe; Henson, Neil J.; Rein, Francisca N.; Smythe, Nathan C.; Trovitch, Ryan J.; Gordon, John C.; Organometallics 33 (2014) 7101–; doi:10.1021/om500909h

data_4084906
_publ_section_title
;
 A New Spin on Cyclooctatetraene (COT) Redox Activity: Low-Spin Iron(I)
 Complexes That Exhibit Antiferromagnetic Coupling to a Singly Reduced
 \h4-COT Ligand
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7101
_journal_paper_doi               10.1021/om500909h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C49 H47 Fe P3'
_chemical_formula_sum            'C49 H47 Fe P3'
_chemical_formula_weight         784.62
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.2960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.839(2)
_cell_length_b                   10.8349(12)
_cell_length_c                   18.785(2)
_cell_measurement_temperature    120(1)
_cell_volume                     3803.3(7)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v1013.6-2 (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36297
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0296P)^2^+2.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                5100
_reflns_number_total             6995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500909h_si_002.cif
_cod_data_source_block           Triphos*FeCOT
_cod_depositor_comments
'Adding full bibliography for 4084905--4084907.cif.'
_cod_database_code               4084906
_shelx_res_checksum              5762
_shelx_hkl_checksum              44942