Synthesis, Structure, and Bonding of d0/fn Metallacarboranes Incorporating the η7-Carboranyl Ligand
Kwoli Chui; Qingchuan Yang; Thomas C. W. Mak; Wai Han Lam; Zhenyang Lin; Zuowei Xie; Journal of the American Chemical Society 122 (2000) 5758–5764; doi:10.1021/ja000188m

data_4116043
_publ_section_title
;
 Synthesis, Structure, and Bonding of d0/fn Metallacarboranes
 Incorporating the \h7-Carboranyl Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5758
_journal_page_last               5764
_journal_paper_doi               10.1021/ja000188m
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C72 H128 B20 Na2 O10 Y2'
_chemical_formula_weight         1593.74
_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                 105.590(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.354(2)
_cell_length_b                   14.3310(19)
_cell_length_c                   19.469(3)
_cell_measurement_temperature    294(2)
_cell_volume                     4395.1(11)
_computing_cell_refinement       'BIOTEX Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'BIOTEX Rigaku'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'IP Rigaku'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10390
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  1.119
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            'pale yellow '
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0118(6)
_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   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          1.441
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1358P)^2^+1.2329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2165
_reflns_number_gt                5164
_reflns_number_total             5920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000188m_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        4395.1(10)
_cod_database_code               4116043