N2 Functionalization at Iron Metallaboratranes
Marc-Etienne Moret; Jonas C. Peters; Journal of the American Chemical Society 133 (2011) 18118–18121; doi:10.1021/ja208675p

data_4107124
_publ_section_title
;
 N2 Functionalization at Iron Metallaboratranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18118
_journal_page_last               18121
_journal_paper_doi               10.1021/ja208675p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C47 H82 B Fe N2 O P3 Si3'
_chemical_formula_weight         934.99
_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                107.196(2)
_cell_angle_beta                 91.580(2)
_cell_angle_gamma                101.338(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0358(4)
_cell_length_b                   12.2087(5)
_cell_length_c                   19.5934(7)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.99
_cell_measurement_theta_min      2.36
_cell_volume                     2685.40(18)
_computing_cell_refinement       'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f 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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            328888
_diffrn_reflns_theta_full        45.88
_diffrn_reflns_theta_max         45.88
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9500
_exptl_absorpt_correction_T_min  0.8341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       blade
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         45761
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.4133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                32378
_reflns_number_total             45761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208675p_si_002_3.cif
_cod_data_source_block           mem127
_cod_original_cell_volume        2685.40(17)
_cod_database_code               4107124