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_1512947
_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            'C32 H62 Ba O20'
_chemical_formula_weight         904.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.939(2)
_cell_angle_beta                 88.563(2)
_cell_angle_gamma                76.781(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0694(9)
_cell_length_b                   8.4231(10)
_cell_length_c                   16.5708(19)
_cell_measurement_reflns_used    8201
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.50
_cell_volume                     1079.5(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       '\w 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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8317
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.8902
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0500P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                3736
_reflns_number_total             3738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-104-108-1.cif
_cod_data_source_block           ba
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512947