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_4104775
_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            'C110 H202 B2 Fe2 N4 O3 P6'
_chemical_formula_weight         1947.90
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.306(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.914(3)
_cell_length_b                   27.596(4)
_cell_length_c                   25.488(4)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.18
_cell_volume                     11103(3)
_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_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1137
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81105
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.9073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         7983
_refine_ls_number_restraints     2064
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.1303
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+367.5974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3042
_refine_ls_wR_factor_ref         0.3120
_reflns_number_gt                6564
_reflns_number_total             7983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903967z_si_002_2.cif
_cod_data_source_block           08318
_cod_database_code               4104775