Formation of Hydroxyindenyl and Vinylidene Ligands by Reaction of Internal Alkynes with Cp*Fe(CO)(NCMe)Ph
Kalman, Steven E.; Gunnoe, T. Brent; Sabat, Michal; Organometallics 33 (2014) 5457–; doi:10.1021/om500748v

data_4084361
_publ_section_title
;
 Formation of Hydroxyindenyl and Vinylidene Ligands by Reaction of
 Internal Alkynes with Cp*Fe(CO)(NCMe)Ph
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5457
_journal_paper_doi               10.1021/om500748v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C25 H38 Fe O Si2'
_chemical_formula_weight         466.58
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 118.007(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.407(9)
_cell_length_b                   18.427(9)
_cell_length_c                   17.500(9)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      3.34
_cell_volume                     5241(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58643
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.343
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10024
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+13.7901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2895
_refine_ls_wR_factor_ref         0.3040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6597
_reflns_number_total             10024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500748v_si_002.cif
_cod_data_source_block           C25H38OSi2Fe
_cod_depositor_comments
;Adding full bibliography for 4084360--4084361.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5241(4)
_cod_database_code               4084361
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.948