Allyl complexes of the heavy alkaline-earth metals: molecular structure and catalytic behavior
Quisenberry, Keith T.; White, Rosemary E.; Hanusa, Timothy P.; Brennessel, William W.; New Journal of Chemistry 34 (2010) 1579–; doi:10.1039/c0nj00084a

data_7053487
_publ_section_title
;
 Allyl complexes of the heavy alkaline-earth metals: molecular structure
 and catalytic behavior
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1579
_journal_paper_doi               10.1039/c0nj00084a
_journal_volume                  34
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C49 H113 Ba2 K O Si10'
_chemical_formula_sum            'C49 H113 Ba2 K O Si10'
_chemical_formula_weight         1313.07
_chemical_name_common            04357
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4705(14)
_cell_length_b                   21.891(3)
_cell_length_c                   30.387(4)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.41
_cell_volume                     7630.2(17)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            91768
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.7346
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
'Flack H D (1983), 7917 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         17485
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+3.8940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                15246
_reflns_number_total             17485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00084a.txt
_cod_data_source_block           04357
_cod_original_cell_volume        7630.2(16)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7053487