Crystal structure of tetranitropalladato(II)tetrakis[(15-crown-5)sodium] tetranitropalladate(II), {[Na(C~10~H~20~O~5~)]~4~Pd(NO~2~)~4~}[Pd (NO~2~)~4~]
Y. Liu; D.-C. Li; J.-M. Dou; D.-Q. Wang; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 191–193; doi:

data_8101731
_publ_section_title
;
Crystal structure of tetranitropalladato(II)tetrakis[(15-crown-5)sodium] 
tetranitropalladate(II), {[Na(C~10~H~20~O~5~)]~4~Pd(NO~2~)~4~}[Pd
(NO~2~)~4~]
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              191
_journal_page_last               193
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         {[Na(15-cr-5)]~4~[Pd(NO~2~)~4~]}[Pd(NO~2~)~2~]
_chemical_formula_sum            'C40 H80 N8 Na4 O36 Pd2'
_chemical_formula_weight         1553.88
_chemical_melting_point          443.1(10)
_chemical_name_systematic
; 
 tetranitropalladato(II)tetrakis[(15-crown-5)sodium] tetranitropalladate(II) 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.036(7)
_cell_angle_beta                 74.511(6)
_cell_angle_gamma                89.404(7)
_cell_formula_units_Z            1
_cell_length_a                   10.530(4)
_cell_length_b                   11.955(5)
_cell_length_c                   13.698(6)
_cell_measurement_reflns_used    2148
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.488
_cell_measurement_theta_min      2.655
_cell_volume                     1655.4(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9529
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.8566
_exptl_absorpt_correction_T_min  0.7319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6510
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                3851
_reflns_number_total             6510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1471.cff
_cod_data_source_block           021228b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '169-171 \%C' was changed to
'443.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1655.5(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101731