ansa-Cyclopentadienyl-Arene Tantalum Complexes: Structure and Reactivity of Neutral, Cationic, and Dicationic Derivatives
Otten, Edwin; Meetsma, Auke; Hessen, Bart; Organometallics 31 (2012) 6071–; doi:10.1021/om300421m

data_4079056
_publ_section_related_literature
;
;
_publ_section_title
;
 ansa-Cyclopentadienyl-Arene Tantalum Complexes: Structure and Reactivity
 of Neutral, Cationic, and Dicationic Derivatives
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6071
_journal_paper_doi               10.1021/om300421m
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C24 H35 O2 Ta, 2(C24 B F20), C4 H8 O'
_chemical_formula_sum            'C76 H43 B2 F40 O3 Ta'
_chemical_formula_weight         1966.68
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2008-03-20  11:56:30'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 110308)
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?

2010-01-14 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 104.323(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.626(3)
_cell_length_b                   14.384(2)
_cell_length_c                   24.493(4)
_cell_measurement_reflns_used    7391
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      2.46
_cell_volume                     7040.8(18)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2007)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-07 (Beurskens et al., 2007)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            57573
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2007).
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.8715
_exptl_absorpt_correction_T_min  0.4189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2007))'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.494
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         15316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                10542
_reflns_number_total             15316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300421m_si_002.cif
_cod_data_source_block           DATNAM
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079056
_vrn_publ_code_number_frames     1800
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    7.9