An Unusual Hydrogen Migration/C-H Activation Reaction with Group 3 Metals
Bryan N. Williams; Diego Benitez; Kevin L. Miller; Ekaterina Tkatchouk; William A. Goddard; Paula L. Diaconescu; Journal of the American Chemical Society 133 (2011) 4680–4683; doi:10.1021/ja110505r

data_4105863
_publ_section_title
;
 An Unusual Hydrogen Migration/C-H Activation Reaction with Group 3 Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4680
_journal_page_last               4683
_journal_paper_doi               10.1021/ja110505r
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'2(C53 H74 Fe N3 O2 Si2 Y), C4 H9, C5 H12, C H3'
_chemical_formula_sum            'C116 H172 Fe2 N6 O4 Si4 Y2'
_chemical_formula_weight         2116.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.8000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.084(2)
_cell_length_b                   17.1073(15)
_cell_length_c                   28.101(3)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      3.69
_cell_volume                     11272.8(18)
_computing_cell_refinement       'Bruker APEX11'
_computing_data_collection       'Bruker APEX11'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            99114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.9225
_exptl_absorpt_correction_T_min  0.8869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         27285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+5.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                17239
_reflns_number_total             27285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110505r_si_002_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        11272.8(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105863