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_7216176
_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         'C20 H18 N2 O6 Pd -2, 2(Na +), H2 O'
_chemical_formula_sum            'C20 H20 N2 Na2 O7 Pd'
_chemical_formula_weight         552.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 124.4800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4083(6)
_cell_length_b                   22.4457(12)
_cell_length_c                   13.4740(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.01
_cell_volume                     4090.6(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23741
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.105
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7475
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0427P)^2^+13.4385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.665
_reflns_number_gt                7363
_reflns_number_total             7475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00669k2.cif
_cod_data_source_block           ff546orang1
_cod_depositor_comments
;
Adding full bibliography for 7216172--7216176.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H40 N4 Na4 O14 Pd2'
_cod_original_formula_weight         1105.52
_cod_original_formula_moiety         'C40 H40 N4 Na4 O14 Pd2'
_cod_original_formula_units_Z            4
_cod_database_code               7216176
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2013-4
_shelx_res_checksum              52076