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_7103700
_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)2(?2-O)(?2-NMe)Ti3(NMe2)
_chemical_formula_sum            'C39.5 H68 B18 N8 O Ti3'
_chemical_formula_weight         1009.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.984(7)
_cell_angle_beta                 82.147(7)
_cell_angle_gamma                80.152(9)
_cell_formula_units_Z            2
_cell_length_a                   12.5957(12)
_cell_length_b                   13.0482(14)
_cell_length_c                   18.3677(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.06
_cell_measurement_theta_min      9.06
_cell_volume                     2918.8(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1673
_diffrn_reflns_av_sigmaI/netI    0.7605
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11997
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        6.73
_diffrn_standards_interval_count 3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11443
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.4496
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_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          0.2339
_refine_ls_wR_factor_ref         0.3296
_reflns_number_gt                2728
_reflns_number_total             11443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301772a.txt
_cod_data_source_block           (DcabNN)2(?2-O)(?2-NMe)Ti3(NMe2)4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_original_formula_sum        'C39.50 H68 B18 N8 O Ti3'
_cod_database_code               7103700