A Photochemical Metallocene Route to Anionic Enediynes: Synthesis, Solid-State Structures, and ab Initio Computations on Cyclopentadienidoenediynes
Joseph M. O'Connor; Kim K. Baldridge; Betsy L. Rodgers; Marissa Aubrey; Ryan L. Holland; W. Scott Kassel; Arnold L. Rheingold; Journal of the American Chemical Society 132 (2010) 11030–11032; doi:10.1021/ja105149k

data_4102849
_publ_section_title
;
 A Photochemical Metallocene Route to Anionic Enediynes: Synthesis,
 Solid-State Structures, and ab Initio Computations on
 Cyclopentadienidoenediynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11030
_journal_page_last               11032
_journal_paper_doi               10.1021/ja105149k
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C16 H14 Fe'
_chemical_formula_sum            'C16 H14 Fe'
_chemical_formula_weight         262.12
_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                89.107(8)
_cell_angle_beta                 78.260(8)
_cell_angle_gamma                75.326(7)
_cell_formula_units_Z            4
_cell_length_a                   10.096(8)
_cell_length_b                   11.064(10)
_cell_length_c                   11.9103(14)
_cell_measurement_reflns_used    3279
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.8
_cell_volume                     1259.2(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3398
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.9122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+1.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                2754
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105149k_si_001.cif
_cod_data_source_block           d
_cod_original_cell_volume        1259.1(15)
_cod_database_code               4102849