Polyol metal complexes. V. Structure of (2,2'-bipyridyl-κ^2^<i>N</i>,<i>N</i>')[<i>meso</i>-oxolane-3,4-diolato(2–)-κ^2^<i>O</i>,<i>O</i>']palladium(II) 6.5-hydrate
Achternbosch, Matthias; Klüfers, Peter; Acta Crystallographica Section C 50 (1994) 175–178; doi:10.1107/S0108270193007322

data_2009496
_publ_section_title
;Polyol metal complexes. V. Structure of
 (2,2'-bipyridyl-\k^2^<i>N</i>,<i>N</i>')[<i>meso</i>-oxolane-3,4-diolato(2--)-\k^2^<i>O</i>,<i>O</i>']palladium(II)
 6.5-hydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              175
_journal_page_last               178
_journal_paper_doi               10.1107/S0108270193007322
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         '[Pd(C4 H6 O3)(C10 H8 N2)],6.5H2 O'
_chemical_formula_structural     '(C10 H8 N2) Pd (C4 H6 O3) (H2 O)6.5'
_chemical_formula_sum            'C14 H27 N2 O9.5 Pd'
_chemical_formula_weight         481.78
_chemical_melting_point          370.15
_chemical_name_systematic
;
2,2'-bipyridyl meso-oxolane-3,4-diolato(2-) palladium(II) 6.5-hydrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.723(3)
_cell_length_b                   15.126(3)
_cell_length_c                   14.796(3)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    221(3)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      10
_cell_volume                     3966.5(13)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) and PLATON (Spek, 1982)
;
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      221(3)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3898
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.7826
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.6136(5)
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.326
_refine_ls_extinction_coef       0.00011(5)
_refine_ls_extinction_method
'F~c~^*^ = kF~c~{1 + 0.001F~c~^2^l^3^[sin(2\q)]^-1^}^-1/4^'
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0266
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0298P)^2^ + 3.0616P] where
  P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0704
_refine_ls_wR_factor_obs         0.0618
_reflns_number_observed          2793
_reflns_number_total             3898
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sh1065.cif
_cod_data_source_block           pdery
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '97_C' was changed to '370.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '97_C' was changed to '370.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2009496