Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 33. Synthesis of Mixed-Ligand Metallacarboranes of Yttrium and Lanthanides Derived from Open η5-Pentadiene and C2B4-Carborane: A Synthetic and Structural Investigation
Wang, Jianhui; Zheng, Chong; Canseco-Melchor, Graciela; Hilby, Daniel J.; Maguire, John A.; Hosmane, Narayan S.; Organometallics 26 (2007) 577–; doi:10.1021/om060751v

data_4072507
_publ_section_title
;
 Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 33. Synthesis
 of Mixed-Ligand Metallacarboranes of Yttrium and Lanthanides Derived from
 Open \h5-Pentadiene and C2B4-Carborane:&#x00A0; A Synthetic and
 Structural Investigation
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              577
_journal_paper_doi               10.1021/om060751v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C15 H33 B4 Gd Si2'
_chemical_formula_weight         470.08
_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                 94.898(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7007(15)
_cell_length_b                   8.4042(8)
_cell_length_c                   16.8002(16)
_cell_measurement_reflns_used    329
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2208.7(4)
_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      203(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16071
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.104
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.431327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.596
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00026(10)
_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   1.574
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.574
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0068P)^2^+6.1197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                3827
_reflns_number_total             3874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060751vsi20061109_052458.cif
_cod_data_source_block           compd_5_hos291
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072507