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_4120408
_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            'C38 H59 B Fe O2 P2 Si2'
_chemical_formula_weight         732.63
_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                90.693(2)
_cell_angle_beta                 103.060(3)
_cell_angle_gamma                90.701(3)
_cell_formula_units_Z            4
_cell_length_a                   12.6336(12)
_cell_length_b                   18.0101(17)
_cell_length_c                   18.2534(13)
_cell_measurement_reflns_used    9546
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.11
_cell_measurement_theta_min      2.26
_cell_volume                     4045.0(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 0.963
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            299923
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.12
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.8632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         39962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                27063
_reflns_number_total             39962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406874k_si_002_6.cif
_cod_data_source_block           dlms114
_cod_database_code               4120408