Ground-State Singlet L3Fe-(μ-N)-FeL3 and L3Fe(NR) Complexes Featuring Pseudotetrahedral Fe(II) Centers
Steven D. Brown; Jonas C. Peters; Journal of the American Chemical Society 127 (2005) 1913–1923; doi:10.1021/ja0453073

data_4111464
_publ_section_title
;
 Ground-State Singlet L3Fe-(\m-N)-FeL3 and L3Fe(NR) Complexes Featuring
 Pseudotetrahedral Fe(II) Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1913
_journal_page_last               1923
_journal_paper_doi               10.1021/ja0453073
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C51 H47 B Fe N3 P3'
_chemical_formula_weight         861.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.2270(10)
_cell_angle_beta                 95.2290(10)
_cell_angle_gamma                111.0900(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0738(10)
_cell_length_b                   14.2209(11)
_cell_length_c                   14.6878(12)
_cell_measurement_reflns_used    6492
_cell_measurement_temperature    96(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.65
_cell_volume                     2128.4(3)
_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      96(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44993
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            opaque
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      0
_exptl_crystal_description       rough
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.809
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.809
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                7839
_reflns_number_total             9998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0453073si20040804_122853_2.cif
_cod_data_source_block           sdb31
_cod_database_code               4111464