Synthesis and Crystal Structure of a “Carbons Apart” Erbacarborane Sandwich: An Example of Novel, One-Pot, Two-Electron Reductive Cage Opening with Concomitant Metalation of the C2B4Carborane Ligand
Wang, Jianhui; Li, Shoujian; Zheng, Chong; Maguire, John A.; Hosmane, Narayan S.; Organometallics 21 (2002) 5149–; doi:10.1021/om020663k

data_4077128
_publ_section_title
;
 Synthesis and Crystal Structure of a &#x201C;Carbons Apart&#x201D;
 Erbacarborane Sandwich:&#x00A0; An Example of Novel, One-Pot,
 Two-Electron Reductive Cage Opening with Concomitant Metalation of the
 C2B4Carborane Ligand
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5149
_journal_paper_doi               10.1021/om020663k
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C24 H60 B8 Er K O2 Si4'
_chemical_formula_weight         785.92
_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                105.006(2)
_cell_angle_beta                 92.473(3)
_cell_angle_gamma                106.286(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5566(18)
_cell_length_b                   12.587(2)
_cell_length_c                   14.955(2)
_cell_measurement_reflns_used    717
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2001.1(5)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Siemens SMART CCD  PLATFORM'
_diffrn_measurement_method       '\w 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  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00000(17)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          3.400
_refine_ls_shift/su_mean         0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.4151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                6565
_reflns_number_total             6856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020663k.cif
_cod_data_source_block           hos181
_cod_original_cell_volume        2001.2(5)
_cod_database_code               4077128