Unexpected retention of the Pd-Ba heterobimetallic structure upon Pd(mu-OOCMe)4Ba(HOOCMe)4 to 18-crown-6 attachment
Sergei E. Nefedov; Elena V. Kushan; Marina A. Uvarova; Natalia Yu. Kozitsyna; Michael N. Vargaftik; Ilya I. Moiseev; Inorganica Chimica Acta 395 (2013) 104–108; doi:10.1016/j.ica.2012.10.008

data_1512949
_publ_section_title
;
 Unexpected retention of the Pd-Ba heterobimetallic structure upon
 Pd(mu-OOCMe)4Ba(HOOCMe)4 to 18-crown-6 attachment
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              104
_journal_page_last               108
_journal_paper_doi               10.1016/j.ica.2012.10.008
_journal_volume                  395
_journal_year                    2013
_chemical_formula_sum            'C20 H38 Ba O15 Pd'
_chemical_formula_weight         762.24
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.330(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.563(4)
_cell_length_b                   18.336(7)
_cell_length_c                   9.128(4)
_cell_measurement_reflns_used    6472
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.50
_cell_volume                     1429.1(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14514
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_T_max  0.8202
_exptl_absorpt_correction_T_min  0.7609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0379
_reflns_number_gt                6333
_reflns_number_total             7292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-104-108-3.cif
_cod_data_source_block           pdbaoh2
_cod_original_cell_volume        1429.1(10)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1512949