Highly Dispersed Pd-SBA15 Materials from Tris(tert-butoxy)siloxy Complexes of Pd(II)
Choi, Yeon S.; Moschetta, Eric G.; Miller, Jeffrey T.; Fasulo, Meg; McMurdo, Meredith J.; Rioux, Robert M.; Tilley, T. Don; ACS Catalysis 1 (2011) 1166–; doi:10.1021/cs2002719

data_4501462
_publ_section_title
;
 Highly Dispersed Pd-SBA15 Materials from Tris(tert-butoxy)siloxy
 Complexes of Pd(II)
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              1166
_journal_paper_doi               10.1021/cs2002719
_journal_volume                  1
_journal_year                    2011
_chemical_formula_moiety         'C42 H78 N2 O8 Pd Si2'
_chemical_formula_sum            'C42 H78 N2 O8 Pd Si2'
_chemical_formula_weight         901.64
_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                 101.799(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.760(3)
_cell_length_b                   24.958(6)
_cell_length_c                   14.913(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      26.923
_cell_measurement_theta_min      2.457
_cell_volume                     5013(2)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      138(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w and \f 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10973
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_correction_T_min  0.9130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.529
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         14237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+7.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                10932
_reflns_number_total             10973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs2002719_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4501462