First structural characterisation of a 2,1,12-MC2B9 metallacarborane, [2,2,2-(NMe2)3-closo-2,1,12-TaC2B9H11]. Trends in boron NMR shifts on replacing a {BH} vertex with a metal {MLn} vertex in icosahedral carboranes
Batsanov, Andrei S.; Eva, Pauline A.; Fox, Mark A.; Howard, Judith A. K.; Hughes, Andrew K.; Johnson, Andrew L.; Martin, Aileen M.; Wade, Ken; Journal of the Chemical Society, Dalton Transactions  (2000) 3519–; doi:10.1039/b005294i

data_7010046
_publ_section_title
;
 First structural characterisation of a 2,1,12-MC2B9 metallacarborane,
 [2,2,2-(NMe2)3-closo-2,1,12-TaC2B9H11]. Trends in boron NMR shifts on
 replacing a {BH} vertex with a metal {MLn} vertex in icosahedral
 carboranes
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3519
_journal_paper_doi               10.1039/b005294i
_journal_year                    2000
_chemical_formula_sum            'C8 H29 B9 N3 Ta'
_chemical_formula_weight         445.58
_chemical_name_systematic
; 
 2,2,2-tris(dimethylamido)-closo-2,1,12-tantalacarborane   
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.04(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.758(1)
_cell_length_b                   17.658(3)
_cell_length_c                   10.326(1)
_cell_measurement_reflns_used    943
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      12.0
_cell_volume                     1769.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  '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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17446
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    6.201
_exptl_absorpt_correction_T_max  0.3693
_exptl_absorpt_correction_T_min  0.2249
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'XPREP (SHELXTL, 1997); before correction R(int'
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombohedral block'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00275(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0164
_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^)+(0.0148P)^2^+1.4100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0366
_reflns_number_gt                4071
_reflns_number_total             4719
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b005294i.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010046