Synthesis, X-ray crystal structure, NMR characterization and theoretical calculations on [Cp2Ta(η2-H2)(CO)]+, the first thermally stable group 5 dihydrogen complex
Sabo-Etienne, Sylviane; Rodriguez, Venancio; Donnadieu, Bruno; Chaudret, Bruno; Abou el Makarim, Hassna; Barthelat, Jean-Claude; Ulrich, Stefan; Limbach, Hans-Heinrich; Moïse, Claude; New Journal of Chemistry 25 (2001) 55–; doi:10.1039/b002073g

data_7051011
_publ_section_title
;
 Synthesis, X-ray crystal structure, NMR characterization and
 theoretical calculations on [Cp2Ta(\h2-H2)(CO)]+, the first thermally
 stable group 5 dihydrogen complex
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              55
_journal_paper_doi               10.1039/b002073g
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         '[C11H12OTa][B(C6H3)(CF3)2]4;1.5(CH2Cl2)'
_chemical_formula_sum            'C44.5 H27 B4 Cl3 F24 O Ta'
_chemical_formula_weight         1331.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 99.40(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00
_cell_length_a                   13.152(2)
_cell_length_b                   18.720(3)
_cell_length_c                   20.918(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.45
_cell_volume                     5081.0(14)
_computing_cell_refinement
'Stoe and Cie (1996) IPDS Manual. Version   2.75. Stoe and Cie, Darmstadt, Germany'
_computing_data_collection
'Stoe and Cie (1996) IPDS Manual. Version   2.75. Stoe and Cie, Darmstadt, Germany'
_computing_data_reduction
'Stoe and Cie (1996) IPDS Manual. Version   2.75. Stoe and Cie, Darmstadt, Germany'
_computing_molecular_graphics
;
CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_detector_area_resol_mean '(1.45 - 24.2)'
_diffrn_measured_fraction_theta_max 93.3%
_diffrn_measurement_device_type
'Stoe and Cie (1996) IPDS Manual. Version   2.75. Stoe and Cie, Darmstadt, Germany'
_diffrn_measurement_method       'rotation en'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK(
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7545
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    24.16
_exptl_absorpt_correction_T_max  0.7620
_exptl_absorpt_correction_T_min  0.5898
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; . 
Absorption corrections were applied on the data by using a set of 
symmetry equivalent reflections selected with the criterion [I>3((I)] 
such that all directions of the reciprocal space are equally represented.
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.74
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' rod '
_exptl_crystal_F_000             2586.05
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.85
_refine_diff_density_min         -1.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   0.9868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           userblock
_refine_ls_number_parameters     694
_refine_ls_number_reflns         6322
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/su_max          0.683701
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0623
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_observed          6322
_reflns_number_total             39337
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            b002073g.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
'/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '120K' was changed to '120' -
the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        5067(2)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7051011
_d(hkl)_range                    '(14.228 - 0.867)'
_absorpt_process_ref
;
 [X-Shape a Crystal Optimisation for Numerical Absorption Corrections 
 Revision 1.01 July 1996 STOE and Cie GMBH 1996]
;
_diffrn_reflns_2theta_min        2.9
_diffrn_reflns_2theta_max        48.4