Well-Defined Iron Catalyst for Improved Hydrogenation of Carbon Dioxide and Bicarbonate
Carolin Ziebart; Christopher Federsel; Pazhamalai Anbarasan; Ralf Jackstell; Wolfgang Baumann; Anke Spannenberg; Matthias Beller; Journal of the American Chemical Society 134 (2012) 20701–20704; doi:10.1021/ja307924a

data_4119035
_publ_section_title
;
 Well-Defined Iron Catalyst for Improved Hydrogenation of Carbon Dioxide
 and Bicarbonate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20701
_journal_page_last               20704
_journal_paper_doi               10.1021/ja307924a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C54 H42 B F5 Fe P4'
_chemical_formula_weight         976.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0906(3)
_cell_length_b                   22.3234(4)
_cell_length_c                   26.9891(5)
_cell_measurement_reflns_used    10053
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.48
_cell_volume                     10296.9(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            78373
_diffrn_reflns_theta_full        26.84
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9509
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
The contribution of disordered solvent was taken into account using
PLATON/SQUEEZE.
;
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10932
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                7482
_reflns_number_total             10932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307924a_si_001.cif
_cod_data_source_block           ks1220
_cod_database_code               4119035