Crystallographic identification of an unusual homoleptic palladium citrate [Na(OH2)6]·{[Na3(OH2)8]3[NaPd3(C6H4O7)3]2}·(H2O) stabilised by intermetallic aggregation with sodium and heavy hydration
Gunari, Parag; s/o Krishnasamy, Suresh; Bai, Shi-Qiang; Hor, T. S. Andy; Dalton Transactions 39 (2010) 9462–; doi:10.1039/c0dt00273a

data_7026213
_publ_section_title
;
 Crystallographic identification of an unusual homoleptic palladium
 citrate [Na(OH2)6]&#x00B7;{[Na3(OH2)8]3[NaPd3(C6H4O7)3]2}&#x00B7;(H2O)
 stabilised by intermetallic aggregation with sodium and heavy hydration
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              9462
_journal_paper_doi               10.1039/c0dt00273a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C18 H43 Na6 O36.5 Pd3'
_chemical_formula_weight         1300.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.8632(6)
_cell_length_b                   15.8632(6)
_cell_length_c                   28.772(2)
_cell_measurement_reflns_used    4515
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.57
_cell_volume                     6270.2(5)
_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      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11706
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_correction_T_min  0.8223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Not Measured'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3882
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.825
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2452
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+146.1366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                2304
_reflns_number_total             2452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00273a.txt
_cod_data_source_block           a7001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6270.1(6)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C18 H43 Na6 O36.50 Pd3'
_cod_database_code               7026213