#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/29/1512948.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1512948
loop_
_publ_author_name
'Sergei E. Nefedov'
'Elena V. Kushan'
'Marina A. Uvarova'
'Natalia Yu. Kozitsyna'
'Michael N. Vargaftik'
'Ilya I. Moiseev'
_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            'C24.5 H54 Ba O14 Pd'
_chemical_formula_weight         816.42
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7761(14)
_cell_length_b                   16.6367(14)
_cell_length_c                   18.8337(18)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.28
_cell_volume                     4003.1(7)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14832
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  0.8427
_exptl_absorpt_correction_T_min  0.7980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         3073
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1100P)²+6.4300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                1766
_reflns_number_total             3073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-104-108-2.cif
_cod_data_source_block           pdba
_cod_original_sg_symbol_H-M      Cmcm
_cod_original_formula_sum        'C24.50 H54 Ba O14 Pd'
_cod_database_code               1512948
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.5000 0.53947(3) 0.7500 0.0526(3) Uani 1 4 d SD . .
Pd1 Pd 0.5000 0.75460(5) 0.7500 0.0634(3) Uani 1 4 d S . .
O1 O 0.3893(5) 0.7591(3) 0.8260(3) 0.0859(16) Uani 1 1 d . A .
O2 O 0.3532(11) 0.6294(8) 0.8172(10) 0.089(4) Uani 0.50 1 d P A 1
O2' O 0.4057(13) 0.6331(7) 0.8507(7) 0.082(4) Uani 0.50 1 d P A 2
C2 C 0.276(3) 0.6961(16) 0.9131(17) 0.083(2) Uani 0.50 1 d P A 1
H2A H 0.3089 0.6783 0.9563 0.125 Uiso 0.50 1 calc PR A 1
H2B H 0.2201 0.6604 0.9011 0.125 Uiso 0.50 1 calc PR A 1
H2C H 0.2495 0.7495 0.9196 0.125 Uiso 0.50 1 calc PR A 1
C2' C 0.282(4) 0.7180(13) 0.912(2) 0.142(15) Uani 0.50 1 d P A 2
H2'A H 0.2116 0.7123 0.8946 0.213 Uiso 0.50 1 calc PR A 2
H2'B H 0.2938 0.7726 0.9259 0.213 Uiso 0.50 1 calc PR A 2
H2'C H 0.2928 0.6829 0.9513 0.213 Uiso 0.50 1 calc PR A 2
C1 C 0.3571(7) 0.6963(5) 0.8533(4) 0.083(2) Uani 1 1 d . . .
O3 O 0.5000 0.4542(11) 0.8940(9) 0.323(18) Uani 1 2 d SD . .
O4 O 0.6722(7) 0.4494(9) 0.8205(6) 0.293(9) Uani 1 1 d D A .
C3 C 0.5852(11) 0.4119(11) 0.9238(8) 0.323(18) Uani 1 1 d D A .
H3A H 0.5813 0.3553 0.9117 0.387 Uiso 1 1 calc R . .
H3B H 0.5852 0.4171 0.9751 0.387 Uiso 1 1 calc R . .
C4 C 0.6774(12) 0.4471(12) 0.8944(7) 0.293(9) Uani 1 1 d D . .
H4A H 0.6855 0.5013 0.9126 0.352 Uiso 1 1 calc R A .
H4B H 0.7381 0.4161 0.9088 0.352 Uiso 1 1 calc R . .
C5 C 0.7663(13) 0.4271(16) 0.7875(8) 0.293(9) Uani 1 1 d D . .
H5A H 0.7848 0.3736 0.8036 0.352 Uiso 1 1 calc R A .
H5B H 0.8208 0.4633 0.8036 0.352 Uiso 1 1 calc R . .
C6 C 0.5000 0.1111(17) 0.7500 0.087(4) Uani 0.50 4 d SP . .
H6A H 0.5000 0.0536 0.7500 0.131 Uiso 0.50 4 d SPR . .
C7 C 0.409(2) 0.1410(11) 0.7500 0.087(4) Uani 0.50 2 d SP . .
H7A H 0.3470 0.1088 0.7500 0.105 Uiso 0.50 2 d SPR . .
C8 C 0.406(2) 0.2254(11) 0.7500 0.087(4) Uani 0.50 2 d SP . .
H8A H 0.3412 0.2548 0.7500 0.105 Uiso 0.50 2 d SPR . .
C9 C 0.5000 0.2639(17) 0.7500 0.087(4) Uani 0.50 4 d SP . .
H9A H 0.4892 0.3210 0.7500 0.131 Uiso 0.25 2 d SPR . .
C10 C 0.5000 -0.077(6) 0.467(5) 0.17(3) Uani 0.25 2 d SPD . .
H10A H 0.5000 -0.1297 0.4461 0.253 Uiso 0.25 2 d SPR . .
C11 C 0.5000 -0.084(2) 0.541(6) 0.17(3) Uani 0.25 2 d SPD . .
H11A H 0.5000 -0.1315 0.5699 0.202 Uiso 0.25 2 d SPR . .
C12 C 0.5000 -0.003(3) 0.561(3) 0.22(6) Uani 0.25 2 d SPD . .
H12A H 0.5000 0.0002 0.6121 0.327 Uiso 0.25 2 d SPR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Ba1 O2 55.6(8) 12_655 3_656
O2 Ba1 O2 87.5(6) 12_655 .
O2 Ba1 O2 113.1(6) 3_656 .
O2 Ba1 O2 113.1(6) 12_655 10_557
O2 Ba1 O2 87.5(6) 3_656 10_557
O2 Ba1 O2 55.6(8) . 10_557
O2 Ba1 O2' 70.5(6) 12_655 .
O2 Ba1 O2' 108.3(3) 3_656 .
O2 Ba1 O2' 19.5(3) . .
O2 Ba1 O2' 72.8(6) 10_557 .
O2 Ba1 O2' 19.5(3) 12_655 12_655
O2 Ba1 O2' 72.8(6) 3_656 12_655
O2 Ba1 O2' 70.5(6) . 12_655
O2 Ba1 O2' 108.3(3) 10_557 12_655
O2' Ba1 O2' 52.3(8) . 12_655
O2 Ba1 O2' 72.8(6) 12_655 3_656
O2 Ba1 O2' 19.5(3) 3_656 3_656
O2 Ba1 O2' 108.3(3) . 3_656
O2 Ba1 O2' 70.5(6) 10_557 3_656
O2' Ba1 O2' 110.5(5) . 3_656
O2' Ba1 O2' 87.8(6) 12_655 3_656
O2 Ba1 O2' 108.3(3) 12_655 10_557
O2 Ba1 O2' 70.5(6) 3_656 10_557
O2 Ba1 O2' 72.8(6) . 10_557
O2 Ba1 O2' 19.5(3) 10_557 10_557
O2' Ba1 O2' 87.8(6) . 10_557
O2' Ba1 O2' 110.5(5) 12_655 10_557
O2' Ba1 O2' 52.3(8) 3_656 10_557
O2 Ba1 O4 63.8(5) 12_655 .
O2 Ba1 O4 88.6(4) 3_656 .
O2 Ba1 O4 125.5(5) . .
O2 Ba1 O4 176.0(4) 10_557 .
O2' Ba1 O4 107.6(4) . .
O2' Ba1 O4 69.6(5) 12_655 .
O2' Ba1 O4 105.7(4) 3_656 .
O2' Ba1 O4 157.3(4) 10_557 .
O2 Ba1 O4 88.6(4) 12_655 10_557
O2 Ba1 O4 63.8(5) 3_656 10_557
O2 Ba1 O4 176.0(4) . 10_557
O2 Ba1 O4 125.5(5) 10_557 10_557
O2' Ba1 O4 157.3(4) . 10_557
O2' Ba1 O4 105.7(4) 12_655 10_557
O2' Ba1 O4 69.6(5) 3_656 10_557
O2' Ba1 O4 107.6(4) 10_557 10_557
O4 Ba1 O4 53.0(5) . 10_557
O2 Ba1 O4 125.5(5) 12_655 12_655
O2 Ba1 O4 176.0(4) 3_656 12_655
O2 Ba1 O4 63.8(5) . 12_655
O2 Ba1 O4 88.6(4) 10_557 12_655
O2' Ba1 O4 69.6(5) . 12_655
O2' Ba1 O4 107.6(4) 12_655 12_655
O2' Ba1 O4 157.3(4) 3_656 12_655
O2' Ba1 O4 105.7(4) 10_557 12_655
O4 Ba1 O4 95.4(4) . 12_655
O4 Ba1 O4 119.5(6) 10_557 12_655
O2 Ba1 O4 176.0(4) 12_655 3_656
O2 Ba1 O4 125.5(5) 3_656 3_656
O2 Ba1 O4 88.6(4) . 3_656
O2 Ba1 O4 63.8(5) 10_557 3_656
O2' Ba1 O4 105.7(4) . 3_656
O2' Ba1 O4 157.3(4) 12_655 3_656
O2' Ba1 O4 107.6(4) 3_656 3_656
O2' Ba1 O4 69.6(5) 10_557 3_656
O4 Ba1 O4 119.5(6) . 3_656
O4 Ba1 O4 95.4(4) 10_557 3_656
O4 Ba1 O4 53.0(5) 12_655 3_656
O1 Pd1 O1 90.6(4) 12_655 3_656
O1 Pd1 O1 89.2(4) 12_655 .
O1 Pd1 O1 175.8(2) 3_656 .
O1 Pd1 O1 175.8(2) 12_655 10_557
O1 Pd1 O1 89.2(4) 3_656 10_557
O1 Pd1 O1 90.6(4) . 10_557
O1 Pd1 Ba1 92.12(12) 12_655 .
O1 Pd1 Ba1 92.12(12) 3_656 .
O1 Pd1 Ba1 92.12(12) . .
O1 Pd1 Ba1 92.12(12) 10_557 .
C1 O1 Pd1 119.9(4) . .
C1 O2 Ba1 133.4(9) . .
C1 O2' Ba1 137.9(9) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
C1 C2' H2'A 109.5 . .
C1 C2' H2'B 109.5 . .
H2'A C2' H2'B 109.5 . .
C1 C2' H2'C 109.5 . .
H2'A C2' H2'C 109.5 . .
H2'B C2' H2'C 109.5 . .
O2' C1 O1 122.8(10) . .
O2' C1 O2 42.7(8) . .
O1 C1 O2 121.1(10) . .
O2' C1 C2' 124.1(13) . .
O1 C1 C2' 108.3(11) . .
O2 C1 C2' 124.1(18) . .
O2' C1 C2 111.8(12) . .
O1 C1 C2 122.3(11) . .
O2 C1 C2 110.8(14) . .
C2' C1 C2 14.1(17) . .
C3 O3 C3 100.9(14) . 12_655
C3 O3 Ba1 125.6(5) . .
C3 O3 Ba1 125.6(5) 12_655 .
C4 O4 C5 113.2(8) . .
C4 O4 Ba1 119.7(9) . .
C5 O4 Ba1 124.7(8) . .
O3 C3 C4 106.2(9) . .
O3 C3 H3A 110.5 . .
C4 C3 H3A 110.5 . .
O3 C3 H3B 110.5 . .
C4 C3 H3B 110.5 . .
H3A C3 H3B 108.7 . .
O4 C4 C3 111.0(10) . .
O4 C4 H4A 109.4 . .
C3 C4 H4A 109.4 . .
O4 C4 H4B 109.4 . .
C3 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
O4 C5 C5 116.3(7) . 10_557
O4 C5 H5A 108.2 . .
C5 C5 H5A 108.2 10_557 .
O4 C5 H5B 108.2 . .
C5 C5 H5B 108.2 10_557 .
H5A C5 H5B 107.4 . .
C7 C6 C7 134(3) 3_656 .
C7 C6 H6A 113.2 3_656 .
C7 C6 H6A 113.2 . .
C6 C7 C8 115(3) . .
C6 C7 H7A 122.9 . .
C8 C7 H7A 122.1 . .
C9 C8 C7 116(2) . .
C9 C8 H8A 121.4 . .
C7 C8 H8A 122.3 . .
C8 C9 C8 124(3) 3_656 .
C8 C9 H9A 126.3 3_656 .
C8 C9 H9A 109.8 . .
C11 C10 C12 116(7) . 9_656
C11 C10 H10A 109.4 . .
C12 C10 H10A 134.2 9_656 .
C12 C11 C10 101(6) . .
C12 C11 H11A 129.6 . .
C10 C11 H11A 129.3 . .
C11 C12 C10 142(4) . 9_656
C11 C12 H12A 109.1 . .
C10 C12 H12A 108.5 9_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 O2 2.712(14) 12_655
Ba1 O2 2.712(14) 3_656
Ba1 O2 2.712(13) .
Ba1 O2 2.712(13) 10_557
Ba1 O2' 2.734(12) .
Ba1 O2' 2.734(12) 12_655
Ba1 O2' 2.734(12) 3_656
Ba1 O2' 2.734(12) 10_557
Ba1 O4 2.975(7) .
Ba1 O4 2.975(7) 10_557
Ba1 O4 2.975(7) 12_655
Ba1 O4 2.975(7) 3_656
Pd1 O1 2.014(6) 12_655
Pd1 O1 2.014(6) 3_656
Pd1 O1 2.014(6) .
Pd1 O1 2.014(6) 10_557
O1 C1 1.234(9) .
O2 C1 1.306(15) .
O2' C1 1.222(13) .
C2 C1 1.53(4) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C2' C1 1.50(4) .
C2' H2'A 0.9600 .
C2' H2'B 0.9600 .
C2' H2'C 0.9600 .
O3 C3 1.412(9) .
O3 C3 1.412(10) 12_655
O4 C4 1.393(9) .
O4 C5 1.403(9) .
C3 C4 1.426(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C5 1.41(3) 10_557
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.26(3) 3_656
C6 C7 1.26(3) .
C6 H6A 0.9578 .
C7 C8 1.41(3) .
C7 H7A 0.9599 .
C8 C9 1.36(3) .
C8 H8A 0.9600 .
C9 C8 1.36(3) 3_656
C9 H9A 0.9601 .
C10 C11 1.4000(10) .
C10 C12 1.43(9) 9_656
C10 H10A 0.9600 .
C11 C12 1.4000(10) .
C11 H11A 0.9602 .
C12 C10 1.43(9) 9_656
C12 H12A 0.9599 .
