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_7027628
_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_formula_sum            'C8 H29 B9 N3 Nb'
_chemical_formula_weight         357.54
_chemical_name_systematic
; 
 tris(dimethylamido)-\h^5^-2,3-dicarbaundecaborane(11) niobium(V) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4562(7)
_cell_length_b                   15.6233(12)
_cell_length_c                   16.9319(10)
_cell_measurement_reflns_used    462
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      12.1
_cell_volume                     3559.6(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      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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28901
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '12 h'
_diffrn_standards_number         491
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.8750
_exptl_absorpt_correction_T_min  0.7320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS program (G.M.Sheldrick, 1996); before correction R(int)=0.086'
_exptl_crystal_colour            yellow
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_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         0.466
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_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(5)
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0053P)^2^+3.4194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_obs         0.0625
_reflns_number_observed          7929
_reflns_number_total             9724
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905075bsup1.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0053P)^2^+3.4194P] 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^)+(0.0053P)^2^+3.4194P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7027628