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_7217352
_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         'C40 H42 N4 O15 Pd2 Rb4'
_chemical_formula_sum            'C40 H42 N4 O15 Pd2 Rb4'
_chemical_formula_weight         1373.45
_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
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_cell_angle_alpha                90
_cell_angle_beta                 124.878(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4305(10)
_cell_length_b                   25.1810(19)
_cell_length_c                   14.1936(7)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.86
_cell_volume                     4817.6(5)
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            76964
_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         26.731
_diffrn_reflns_theta_min         1.617
_exptl_absorpt_coefficient_mu    4.830
_exptl_absorpt_correction_T_max  0.0285
_exptl_absorpt_correction_T_min  0.0104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.218
_refine_diff_density_min         -3.262
_refine_diff_density_rms         0.272
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.139(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10045
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1685P)^2^+8.7702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9770
_reflns_number_total             10045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7216174
_cod_data_source_file            c4ce00669k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7217352
_shelx_estimated_absorpt_t_min   0.378
_shelx_estimated_absorpt_t_max   0.595
_shelxl_version_number           2013-4
_shelx_res_checksum              56386