Tetraallyl (2,2'-bipyridyl)-<i>rac</i>-3,3,7,7-tetramethyl-<i>trans</i>-5-palladatricyclo[4.1.0.0^2,^^4^]heptane-1,2,4,6-tetracarboxylate above and below the phase-transition temperature of 194K
Bats, Jan W.; Rivas Nass, Andreas; Hashmi, A. Stephen K.; Acta Crystallographica Section C 56 (2000) 814–817; doi:10.1107/S0108270100006193

data_2011114
_publ_section_title
;Tetraallyl
 (2,2'-bipyridyl)-<i>rac</i>-3,3,7,7-tetramethyl-<i>trans</i>-5-palladatricyclo[4.1.0.0^2,^^4^]heptane-1,2,4,6-tetracarboxylate
 above and below the phase-transition temperature of 194K
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              814
_journal_page_last               817
_journal_paper_doi               10.1107/S0108270100006193
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Pd(C10 H8 N2 )(C26 H32 O8 )]'
_chemical_formula_moiety         'C36 H40 N2 O8 Pd'
_chemical_formula_sum            'C36 H40 N2 O8 Pd'
_chemical_formula_weight         735.10
_chemical_name_systematic
;
tetraallyl (2,2'-bipyridyl)-rac-3,3,7,7-tetramethyl-trans-5-palladatricyclo
[4.1.0.0^2,4^]heptane-1,2,4,6-tetracarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                95.641(12)
_cell_angle_beta                 97.375(11)
_cell_angle_gamma                93.083(9)
_cell_formula_units_Z            4
_cell_length_a                   9.0197(6)
_cell_length_b                   17.918(2)
_cell_length_c                   21.375(3)
_cell_measurement_reflns_used    276
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     3401.6(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'CIF in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS96 (Sheldrick, 1996)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full .901
_diffrn_measured_fraction_theta_max .901
_diffrn_measurement_device_type  SIEMENS_SMART
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0591
_diffrn_reflns_av_sigmaI/netI    .0610
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64204
_diffrn_reflns_theta_full        32.20
_diffrn_reflns_theta_max         32.20
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         703
_exptl_absorpt_coefficient_mu    .599
_exptl_absorpt_correction_T_max  .9768
_exptl_absorpt_correction_T_min  .8166
_exptl_absorpt_correction_type   'numerical (SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          .44
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .04
_refine_diff_density_max         .563
_refine_diff_density_min         -.610
_refine_ls_extinction_coef       .00053(14)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         22046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          .0790
_refine_ls_R_factor_gt           .0459
_refine_ls_shift/su_max          .010
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.04P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1009
_reflns_number_gt                16183
_reflns_number_total             22046
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1601.cif
_cod_data_source_block           I143K
_cod_original_cell_volume        3401.7(7)
_cod_database_code               2011114
_cod_database_fobs_code          2011114