Cyclometallated compounds. XV. A tetranuclear acetate-bridged cyclopalladated molecular box
O'Keefe, Brendan J.; Steel, Peter J.; Acta Crystallographica Section C 56 (2000) 1440–1441; doi:10.1107/S0108270100011768

data_2011600
_publ_section_title
;
 Cyclometallated compounds. XV. A tetranuclear acetate-bridged
 cyclopalladated molecular box
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1440
_journal_page_last               1441
_journal_paper_doi               10.1107/S0108270100011768
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'[Pd4 (C16 H10 N2 O2)2 (C2 H3 O2)4] , 2C H Cl3 , 2H2 O'
_chemical_formula_moiety         'C40 H32 N4 O12 Pd4 , 2C1 H1 Cl3 , 2H2 O'
_chemical_formula_sum            'C42 H38 Cl6 N4 O14 Pd4'
_chemical_formula_weight         1461.06
_chemical_name_systematic
;
tetra-\m-acetato-O:O'-bis{[\m-1,4-bis(2-pyridyloxy)phenylene-N,C^2^:N',C^6^]
dipalladium(II)} bis(trichloromethane) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.797(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.225(5)
_cell_length_b                   15.052(5)
_cell_length_c                   14.135(5)
_cell_measurement_reflns_used    6111
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.15
_cell_volume                     2599.7(16)
_computing_cell_refinement       'SAINT (Siemens 1999)'
_computing_data_collection       'SMART (Siemens 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXL97
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full .991
_diffrn_measured_fraction_theta_max .991
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'Exposures over 0.5\% \f or \w rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .089
_diffrn_reflns_av_sigmaI/netI    .073
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26967
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.735
_exptl_absorpt_correction_T_max  .934
_exptl_absorpt_correction_T_min  .559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Siemens, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .04
_refine_diff_density_max         .96
_refine_diff_density_min         -.95
_refine_ls_extinction_coef       .0010(3)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          .095
_refine_ls_R_factor_gt           .050
_refine_ls_shift/su_max          .027
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0748P)^2^+0.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .134
_reflns_number_gt                3476
_reflns_number_total             5261
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            de1153.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2011600
_cod_database_fobs_code          2011600