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_4076944
_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            'C21 H42 B11 N3 Zr'
_chemical_formula_weight         546.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 110.804(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4363(8)
_cell_length_b                   15.829(1)
_cell_length_c                   10.5619(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1474.74(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9888
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7770
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.56
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.0000(7)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          1.564
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                5932
_reflns_number_total             6170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020325j.cif
_cod_data_source_block           compound_2
_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        1474.8(2)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4076944