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_4079062
_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            'C49 H66 B11 Cl Ge N2 O P2 Pd'
_chemical_formula_weight         1094.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8523(12)
_cell_length_b                   23.421(5)
_cell_length_c                   21.169(3)
_cell_measurement_temperature    173(2)
_cell_volume                     5380.6(15)
_computing_cell_refinement       x-Area
_computing_data_collection       x-Area
_computing_data_reduction        x-Area
_computing_molecular_graphics    'ortep for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            93982
_diffrn_reflns_theta_full        29.19
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.8872
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'x-red, x-shape'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.508
_refine_diff_density_rms         0.263
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.464(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         14366
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0708P)^2^+0.2142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                13244
_reflns_number_total             14366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300438x_si_001.cif
_cod_data_source_block           jd66
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4079062