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_4079061
_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_moiety
'C39 H42 B11 Cl2 O P2 Pd Sn, C12 H28 N, 3(C4 H10 O)'
_chemical_formula_sum            'C63 H100 B11 Cl2 N O4 P2 Pd Sn'
_chemical_formula_weight         1412.30
_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   calculated
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.057(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2731(12)
_cell_length_b                   14.3171(7)
_cell_length_c                   25.7675(14)
_cell_measurement_temperature    173(2)
_cell_volume                     7150.1(7)
_computing_cell_refinement       x-Area
_computing_data_collection       x-Area
_computing_data_reduction        x-Area
_computing_molecular_graphics    platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '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  0.1379
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59464
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.9094
_exptl_absorpt_correction_T_min  0.7759
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'x-red, x-shape'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.3020
_exptl_crystal_size_mid          0.3018
_exptl_crystal_size_min          0.1799
_refine_diff_density_max         1.732
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0900
_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^)+(0.0525P)^2^+44.2847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                9670
_reflns_number_total             13295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300438x_si_001.cif
_cod_data_source_block           hornung80
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079061