A chromotropic PtIIPdIICoII coordination polymer with dual electrocatalytic activity for water reduction and oxidation
San Esteban, Anna Carissa M.; Kuwamura, Naoto; Yoshinari, Nobuto; Konno, Takumi; Dalton Transactions  (2021) –; doi:10.1039/D1DT02587B

data_7708458
_publ_section_title
;
 A chromotropic PtIIPdIICoII coordination polymer with dual
 electrocatalytic activity for water reduction and oxidation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02587B
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C20 H60 Co2 N8 O14 Pd2 Pt2 S4,  Cl4 [+16(H2O)]'
_chemical_formula_sum            'C20 H92 Cl4 Co2 N8 O30 Pd2 Pt2 S4'
_chemical_formula_weight         1915.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0942(2)
_cell_length_b                   21.9908(5)
_cell_length_c                   30.830(8)
_cell_measurement_reflns_used    19848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6820
_cell_measurement_theta_min      1.8470
_cell_volume                     6165.7(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.7479
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     26.00  76.00   0.50    0.62    --   12.17-142.00  61.00  100
  2  \w     27.00  52.00   0.50    0.62    --   12.17 -99.00  90.00   50
  3  \w      8.00  44.00   0.50    0.62    --   12.17  17.00-108.00   72
  4  \w    -68.00  22.00   0.50    0.62    --   12.17 -17.00  82.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0003708000
_diffrn_orient_matrix_UB_12      -0.0072952000
_diffrn_orient_matrix_UB_13      -0.0224078000
_diffrn_orient_matrix_UB_21      0.0778941000
_diffrn_orient_matrix_UB_22      0.0017005000
_diffrn_orient_matrix_UB_23      -0.0001527000
_diffrn_orient_matrix_UB_31      0.0041633000
_diffrn_orient_matrix_UB_32      -0.0313754000
_diffrn_orient_matrix_UB_33      0.0051835000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            35838
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.748
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.7210
_diffrn_reflns_theta_min         1.8521
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.007
_exptl_absorpt_correction_T_max  0.64832
_exptl_absorpt_correction_T_min  0.64098
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_description       plate
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         2.432
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details
;
 Flack x determined using 4200 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         14334
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.700
_reflns_number_gt                11550
_reflns_number_total             14334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02587b2.cif
_cod_data_source_block           2Cl
_cod_database_code               7708458
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.447
_shelx_estimated_absorpt_t_max   0.840
_exptl_absorpt_special_details
;
It was not possible to apply the face indexed absorption correction because 
the video images of the crystal employed were unclear.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.791
_oxdiff_exptl_absorpt_empirical_full_max 1.389
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              60325
_shelx_hkl_checksum              62254
_shelx_fab_checksum              2666