Novel titanium complexes of a multidentate dicarbollide ligand. Synthesis and structural characterization of a constrained geometry complex
Lee, Young-Joo; Lee, Jong-Dae; Ko, Jaejung; Kim, Sang-Hern; Kang, Sang Ook; Chemical Communications (Cambridge, United Kingdom)  (2003) 1364–1365; doi:10.1039/b301772a

data_7113720
_publ_section_title
;
 Novel titanium complexes of a multidentate dicarbollide ligand. Synthesis
 and structural characterization of a constrained geometry complex
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   12
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1364
_journal_page_last               1365
_journal_paper_doi               10.1039/b301772a
_journal_year                    2003
_chemical_formula_moiety         (DcabNN)Ti(NMe2)
_chemical_formula_sum            'C12 H37 B9 N4 Ti'
_chemical_formula_weight         382.65
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.438(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2029(13)
_cell_length_b                   15.714(2)
_cell_length_c                   14.790(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2136.9(5)
_computing_cell_refinement
'SMART Area-Detector Software Package (Bruker AXS, 1995)'
_computing_data_collection
'SMART Area-Detector Software Package (Bruker AXS, 1995)'
_computing_data_reduction
'XPREP: part of SHELXTL 5.04(Bruker AXS, 1995)'
_computing_molecular_graphics    'ORTEP3 (Jonson & Burrett, 1998)'
_computing_publication_material  SHELXL-97(Sheldrick,1997)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type
'Bruker SMART diffractometer/CCD area detector'
_diffrn_measurement_method       \w/2wq
_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  0.1002
_diffrn_reflns_av_sigmaI/netI    0.1366
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11211
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                2050
_reflns_number_total             3982
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103699
_cod_data_source_file            b301772a.txt
_cod_data_source_block           (DcabNN)Ti(NMe2)2
_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/retrospective/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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+0.0000P] 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^)+(0.0788P)^2^+0.0000P] 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        2137.0(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7113720