A CO-Derived Iron Dicarbyne That Releases Olefin upon Hydrogenation
Daniel L. M. Suess; Jonas C. Peters; Journal of the American Chemical Society 135 (2013) 12580–12583; doi:10.1021/ja406874k

data_4120407
_publ_section_title
;
 A CO-Derived Iron Dicarbyne That Releases Olefin upon Hydrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12580
_journal_page_last               12583
_journal_paper_doi               10.1021/ja406874k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C92 H129 B Fe K2 O23 P2'
_chemical_formula_weight         1809.76
_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                96.728(4)
_cell_angle_beta                 96.954(2)
_cell_angle_gamma                115.227(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3954(14)
_cell_length_b                   14.7510(12)
_cell_length_c                   24.5846(14)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.65
_cell_measurement_theta_min      2.55
_cell_volume                     4604.3(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V7.68A (Bruker-AXS, 2007)'
_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 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            340219
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         42.89
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_correction_T_min  0.8995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         64746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.1186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                44074
_reflns_number_total             64746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406874k_si_002_5.cif
_cod_data_source_block           dlms104
_cod_original_formula_sum        'C46 H64.50 B0.50 Fe0.50 K O11.50 P'
_cod_database_code               4120407