Synthesis, Structure, and Reactivity of Group 4 Metallacarboranes Bearing the Ligand [Me2C(C9H6)(C2B9H10)]3−
Liu, Dongmei; Wang, Yaorong; Chan, Hoi-Shan; Tang, Yong; Xie, Zuowei; Organometallics 27 (2008) 5295–; doi:10.1021/om800452f

data_4071891
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Group 4 Metallacarboranes Bearing
 the Ligand [Me2C(C9H6)(C2B9H10)]3&#x2212;
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5295
_journal_paper_doi               10.1021/om800452f
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C33 H59 B9 Cl Na O6 Zr'
_chemical_formula_weight         798.75
_chemical_name_systematic
; 
 ? 
;
_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                78.22(3)
_cell_angle_beta                 83.36(3)
_cell_angle_gamma                84.01(3)
_cell_formula_units_Z            2
_cell_length_a                   12.265(3)
_cell_length_b                   13.110(3)
_cell_length_c                   13.761(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2144.1(9)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.689
_diffrn_measured_fraction_theta_max 0.689
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5695
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                4619
_reflns_number_total             5695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800452f_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        2144.1(7)
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               4071891