Germa- and Stanna-closo-dodecaborate in Reaction with [PdCl2(Xantphos)]: P‒C and B‒H Bond Activation
Dimmer, Jörg-Alexander; Hornung, Martin; Wütz, Tobias; Wesemann, Lars; Organometallics 31 (2012) 7044–; doi:10.1021/om300438x

data_4079065
_publ_section_title
;
 Germa- and Stanna-closo-dodecaborate in Reaction with [PdCl2(Xantphos)]:
 P--C and B--H Bond Activation
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7044
_journal_paper_doi               10.1021/om300438x
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C79.5 H86.5 B11 N2.5 O4.5 P4 Pd2 Sn'
_chemical_formula_weight         1723.29
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.110(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2954(6)
_cell_length_b                   23.7892(10)
_cell_length_c                   21.3124(9)
_cell_measurement_reflns_used    342
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      28.3356
_cell_measurement_theta_min      1.8836
_cell_volume                     7753.4(6)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'omega scans, phi scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            86016
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.86
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.830
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         15229
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0400P)^2^+7.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                11499
_reflns_number_total             15229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300438x_si_001.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C79.50 H86.50 B11 N2.50 O4.50 P4 Pd2 Sn'
_cod_database_code               4079065