Trapping Unstable Terminal Ta-O Multiple Bonds of Monocyclopentadienyl Tantalum Complexes with a Lewis Acid
Sánchez-Nieves, Javier; Frutos, Luis M.; Royo, Pascual; Castaño, Obis; Herdtweck, Eberhardt; Organometallics 24 (2005) 2004–2007; doi:10.1021/om049012+

data_4060302
_publ_section_title
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 Trapping Unstable Terminal Ta-O Multiple Bonds of Monocyclopentadienyl
 Tantalum Complexes with a Lewis Acid
;
_journal_coden_ASTM              ORGND7
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2004
_journal_page_last               2007
_journal_paper_doi               10.1021/om049012+
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C28 H15 B Cl2 F15 O Ta'
_chemical_formula_sum            'C28 H15 B Cl2 F15 O Ta'
_chemical_formula_weight         915.06
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.8081(5)
_cell_angle_beta                 69.2081(5)
_cell_angle_gamma                74.7048(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6113(1)
_cell_length_b                   11.2399(1)
_cell_length_c                   13.7102(2)
_cell_measurement_reflns_used    5366
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.57
_cell_volume                     1469.76(3)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33311
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.041
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_exptl_special_details
;
Diffractometer operator             E. Herdtweck
scanspeed                           2 x 10 s per film
repetition                                 1
dx                                        40
1167 films measured in 10 data sets
set 1:            phi-scan with delta_phi = 1.0
set 2 to 10:  omega-scans with delta_omega = 1.0
;
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.092
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0226
_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^)+(Fo^2^)+(0.0309P)^2^+2.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                5226
_reflns_number_total             5385
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om049012+rom20050126_102307.cif
_cod_data_source_block           ROYN-4250-173
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4060302