Group 5 hydride and borohydride complexes supported by cyclopentadienyl-imido ligand sets.
McLeod, Nicolas A.; Kuzmina, Lyudmila G.; Churakov, Andrei V.; Mountford, Philip; Nikonov, Georgii I.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 188–195; doi:10.1039/c3dt52489b

data_7029241
_publ_section_title
;
 Group 5 hydride and borohydride complexes supported by
 cyclopentadienyl-imido ligand sets.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              188
_journal_page_last               195
_journal_paper_doi               10.1039/c3dt52489b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H52 B2 N2 Ta2'
_chemical_formula_sum            'C34 H52 B2 N2 Ta2'
_chemical_formula_weight         872.32
_chemical_name_systematic
;
[CpTa(u-NAr)(BH4)]2
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.4877(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6770(2)
_cell_length_b                   20.3428(2)
_cell_length_c                   15.7568(2)
_cell_measurement_reflns_used    55248
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     3400.46(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            55248
_diffrn_reflns_theta_full        27.482
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         5.128
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.455
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.40
_refine_diff_density_min         -1.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0738
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5841
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.0030621
_refine_ls_shift/su_mean         0.0000344
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.279 0.129 0.872E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0502
_refine_ls_wR_factor_gt          0.0291
_refine_ls_wR_factor_ref         0.0291
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6198
_reflns_number_total             7965
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0256
_oxford_refine_ls_scale          0.08465(7)
_oxford_reflns_number_all        7740
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3dt52489b.txt
_cod_data_source_block           compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7029241