Synthesis, Structural Characterization, and Reactivity of Group 4 Metallacarboranes Containing the Ligand [Me2C(C5H4)(C2B9H10)]3−
Wang, Yaorong; Liu, Dongmei; Chan, Hoi-Shan; Xie, Zuowei; Organometallics 27 (2008) 2825–; doi:10.1021/om800235w

data_4071570
_publ_section_title
;
 Synthesis, Structural Characterization, and Reactivity of Group 4
 Metallacarboranes Containing the Ligand [Me2C(C5H4)(C2B9H10)]3&#x2212;
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2825
_journal_paper_doi               10.1021/om800235w
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C23 H44 B9 Cl Na O4 Zr'
_chemical_formula_weight         631.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.6620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3272(9)
_cell_length_b                   11.6787(7)
_cell_length_c                   19.0496(11)
_cell_measurement_temperature    293(2)
_cell_volume                     3301.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21934
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.828383
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                6005
_reflns_number_total             7975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800235w-file004.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071570