Synthesis, Structural Characterization, and Reactivity of 13-Vertex Lanthanacarboranes Bearing η7-arachno-Carboranyl Ligands
Cheung, Mak-Shuen; Chan, Hoi-Shan; Xie, Zuowei; Organometallics 24 (2005) 4468–; doi:10.1021/om050417j

data_4076225
_publ_section_title
;
 Synthesis, Structural Characterization, and Reactivity of 13-Vertex
 Lanthanacarboranes Bearing \h7-arachno-Carboranyl Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4468
_journal_paper_doi               10.1021/om050417j
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C30 H76 B20 Er2 N4 Na2 O4'
_chemical_formula_weight         1153.65
_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                112.64(3)
_cell_angle_beta                 96.47(3)
_cell_angle_gamma                110.51(3)
_cell_formula_units_Z            1
_cell_length_a                   9.787(2)
_cell_length_b                   12.471(3)
_cell_length_c                   12.604(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1274.1(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.325
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7925
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.418
_refine_diff_density_min         -2.376
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+3.6449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3849
_reflns_number_total             4480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tom050489si20050526_050851.cif
_cod_data_source_block           9
_cod_original_cell_volume        1274.1(4)
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               4076225