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_7103698
_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)H2
_chemical_formula_sum            'C8 H27 B9 N2'
_chemical_formula_weight         248.61
_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                 99.485(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3868(5)
_cell_length_b                   17.6878(8)
_cell_length_c                   10.6643(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.47
_cell_measurement_theta_min      10.00
_cell_volume                     1560.36(18)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1988)'
_computing_data_reduction        'Xtal3.2 (Hall & Stewart, 1992)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3308
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_count 3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7784
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2070
_reflns_number_gt                2013
_reflns_number_total             3061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301772a.txt
_cod_data_source_block           (DcabNN)H2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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_sg_symbol_H-M      P21/n
_cod_database_code               7103698