Characterization of Structurally Unusual Diiron NxHy Complexes
Caroline T. Saouma; Peter Müller; Jonas C. Peters; Journal of the American Chemical Society 131 (2009) 10358–10359; doi:10.1021/ja903967z

data_4104777
_publ_section_title
;
 Characterization of Structurally Unusual Diiron NxHy Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10358
_journal_page_last               10359
_journal_paper_doi               10.1021/ja903967z
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C108 H104 B2 Fe2 N4 P6'
_chemical_formula_weight         1777.09
_chemical_name_systematic
; 
 ? 
;
_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                95.483(4)
_cell_angle_beta                 95.884(4)
_cell_angle_gamma                118.639(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5700(17)
_cell_length_b                   13.8818(19)
_cell_length_c                   28.049(5)
_cell_measurement_reflns_used    4580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.22
_cell_volume                     4549.1(12)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75437
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1603
_refine_ls_number_reflns         17915
_refine_ls_number_restraints     7915
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0948P)^2^+5.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2050
_reflns_number_gt                11080
_reflns_number_total             17915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903967z_si_002_4.cif
_cod_data_source_block           08348
_cod_database_code               4104777