Bis(tetra-<i>n</i>-butylammonium) di-μ-chloro-bis[(tetramethyl buta-1,3-diene-1,2,3,4-tetracarboxylato-κ^2^<i>C</i>^1^,<i>C</i>^4^)palladium]
Pérez, José; García, Luis; Serrano, Jose Luis; Pérez, Eduardo; Sánchez, Gregorio; Vives, Jorge; Acta Crystallographica Section C 58 (2002) m404–m406; doi:10.1107/S0108270102009642

data_2012820
_publ_section_title
;Bis(tetra-<i>n</i>-butylammonium) di-\m-chloro-bis[(tetramethyl
 buta-1,3-diene-1,2,3,4-tetracarboxylato-\k^2^<i>C</i>^1^,<i>C</i>^4^)palladium]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m404
_journal_page_last               m406
_journal_paper_doi               10.1107/S0108270102009642
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C16 H36 N)2 [Pd2 (C12 H12 O8)2 Cl2]'
_chemical_formula_moiety         '2C16 H36 N 1+ , C24 H24 Cl2 O16 Pd2 2-'
_chemical_formula_sum            'C56 H96 Cl2 N2 O16 Pd2'
_chemical_formula_weight         1337.05
_chemical_name_systematic
;
Bis(tetra-n-butylammonium) di-\m-chloro-bis[(tetramethyl
buta-1,3-diene-1,2,3,4-tetracarboxylato-\k^2^C^1^,C^4^)palladium(0)]
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_cell_angle_alpha                95.929(5)
_cell_angle_beta                 106.777(5)
_cell_angle_gamma                104.100(5)
_cell_formula_units_Z            1
_cell_length_a                   9.5024(6)
_cell_length_b                   12.6678(7)
_cell_length_c                   14.6370(10)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      9.75
_cell_volume                     1607.25(19)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11249
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        4.3
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.055
_reflns_number_gt                5057
_reflns_number_total             5644
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1139.cif
_cod_data_source_block           I
_cod_database_code               2012820
_cod_database_fobs_code          2012820