Transition metal dicarbollide complexes: synthesis, molecular, crystal and electronic structures of [M(C2B9H11)(NMe2)3] (M = Nb or Ta) and their insertion reactions with CO2 and CS2 †
Batsanov, Andrei S.; Churakov, Andrei V.; Howard, Judith A. K.; Hughes, Andrew K.; Johnson, Andrew L.; Kingsley, Andrew J.; Neretin, Ivan S.; Wade, Ken; Journal of the Chemical Society, Dalton Transactions  (1999) 3867–; doi:10.1039/a905075b

data_7027631
_publ_section_title
;
 Transition metal dicarbollide complexes: synthesis, molecular, crystal
 and electronic structures of [M(C2B9H11)(NMe2)3] (M&#x2005;=&#x2005;Nb or
 Ta) and their insertion reactions with CO2 and CS2&#x200A;&#x2020;
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3867
_journal_paper_doi               10.1039/a905075b
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C11 H29 B9 N3 O6 Ta,(C7 H8)0.5'
_chemical_formula_sum            'C14.5 H33 B9 N3 O6 Ta'
_chemical_formula_weight         623.68
_chemical_name_systematic
; 
 tris(N,N-dimethylcarbamato-O,O')-\h^5^-2,3-dicarbaundecaborane(11)-
 tantalum(V) hemi-toluene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.34(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.297(2)
_cell_length_b                   17.424(3)
_cell_length_c                   13.308(3)
_cell_measurement_reflns_used    330
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      12.09
_cell_volume                     2655.9(13)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'SMART 1K CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17271
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    4.172
_exptl_absorpt_correction_T_max  0.5630
_exptl_absorpt_correction_T_min  0.2978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS program (G.M.Sheldrick, 1996); before correction R(int)=0.122'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_obs          0.0329
_refine_ls_shift/esd_max         -0.056
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.1033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0978
_refine_ls_wR_factor_obs         0.0858
_reflns_number_observed          4715
_reflns_number_total             6091
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905075bsup1.cif
_cod_data_source_block           (7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.1033P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.1033P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2655.9(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C14.50 H33 B9 N3 O6 Ta'
_cod_database_code               7027631