Solid-state cis‒trans isomerism in bis(oxamato)palladate(ii) complexes: synthesis, structural studies and catalytic activity
Fortea-Pérez, Francisco R.; Marino, Nadia; Armentano, Donatella; De Munno, Giovanni; Julve, Miguel; Stiriba, Salah-Eddine; CrystEngComm 16 (2014) 6971–; doi:10.1039/C4CE00669K

data_7217353
_publ_section_title
;
 Solid-state cis--trans isomerism in bis(oxamato)palladate(ii) complexes:
 synthesis, structural studies and catalytic activity
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              6971
_journal_paper_doi               10.1039/C4CE00669K
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C60 H74 Cs6 N6 O28 Pd3'
_chemical_formula_sum            'C60 H74 Cs6 N6 O28 Pd3'
_chemical_formula_weight         2443.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.874(5)
_cell_length_b                   24.355(5)
_cell_length_c                   26.539(5)
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.24
_cell_volume                     16077(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            358776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.535
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_description       PARALLELEPIPED
_exptl_crystal_F_000             9344
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.025
_refine_diff_density_min         -4.547
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         17069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1674P)^2^+29.3079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11235
_reflns_number_total             17069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7216175
_cod_data_source_file            c4ce00669k2.cif
_cod_data_source_block           4
_cod_original_cell_volume        16078(6)
_cod_database_code               7217353
_shelx_estimated_absorpt_t_min   0.407
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              23357