A platinum(ii)-palladium(ii)-nickel(ii) heterotrimetallic coordination polymer showing a cooperative effect on catalytic hydrogen evolution.
Kuwamura, Naoto; Kurioka, Yoshinari; Konno, Takumi; Chemical communications (Cambridge, England) 53 (2017) 846–849; doi:10.1039/c6cc08789b

data_7119404
_publ_section_title
;
 A platinum(ii)-palladium(ii)-nickel(ii) heterotrimetallic coordination
 polymer showing a cooperative effect on catalytic hydrogen evolution.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              846
_journal_page_last               849
_journal_paper_doi               10.1039/c6cc08789b
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C20 H52 Cl4 N8 O8 Pd2 Pt2 S4, 6.5(O)'
_chemical_formula_sum            'C20 H52 Cl4 N8 O14.5 Pd2 Pt2 S4'
_chemical_formula_weight         1509.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.206(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.407(4)
_cell_length_b                   23.902(9)
_cell_length_c                   14.901(3)
_cell_measurement_reflns_used    251
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      5.86
_cell_volume                     5689(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22339
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.052
_exptl_absorpt_coefficient_mu    5.910
_exptl_absorpt_correction_T_max  0.182
_exptl_absorpt_correction_T_min  0.105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, ????)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.182
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Flack x determined using 5042 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+7.2795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.902
_reflns_number_gt                11868
_reflns_number_total             12428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08789b2.cif
_cod_data_source_block           PtPd_Konno
_cod_original_formula_sum        'C20 H52 Cl4 N8 O14.50 Pd2 Pt2 S4'
_cod_database_code               7119404
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.384
_shelx_estimated_absorpt_t_max   0.471
_shelx_res_checksum              79221
_shelx_hkl_checksum              32515