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_4084360
_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            'C21 H26 Fe O'
_chemical_formula_weight         350.27
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 94.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.349(2)
_cell_length_b                   8.6120(9)
_cell_length_c                   22.556(2)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      3.33
_cell_volume                     3552.4(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            83309
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.076
_diffrn_reflns_theta_min         3.534
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         15628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+2.4649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10306
_reflns_number_total             15628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500748v_si_002.cif
_cod_data_source_block           C21H26OFe
_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        3552.3(7)
_cod_database_code               4084360
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.935