Synthesis, Structural Characterization, and Catalytic Property of Group 4 Metal Carborane Compounds with aiPr2NB-Bridged Constrained-Geometry Ligand
Zi, Guofu; Li, Hung-Wing; Xie, Zuowei; Organometallics 21 (2002) 3850–; doi:10.1021/om020325j

data_4076943
_publ_section_title
;
 Synthesis, Structural Characterization, and Catalytic Property of Group 4
 Metal Carborane Compounds with aiPr2NB-Bridged Constrained-Geometry
 Ligand
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3850
_journal_paper_doi               10.1021/om020325j
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C8 H30 B9 N3 Ti'
_chemical_formula_weight         313.54
_chemical_name_systematic
; 
 ? 
;
_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                 105.145(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8470(8)
_cell_length_b                   12.298(1)
_cell_length_c                   16.931(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1778.1(3)
_computing_cell_refinement       'Bruker SMART CCD Diffractometer'
_computing_data_collection       'Bruker SMART CCD Diffractometer'
_computing_data_reduction        'Bruker SMART CCD Diffractometer'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD Diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11618
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6142
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0000(12)
_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   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          1.303
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1095P)^2^+0.3470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                3587
_reflns_number_total             4318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020325j.cif
_cod_data_source_block           compound_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1778.2(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076943