Self-assembled multicomponent Pd6 aggregates showing low-humidity proton conduction
Dipak Samanta; Partha Sarathi Mukherjee; Chem.Commun. 50 (2014) 1595–; doi:10.1039/c3cc47965j

data_7111858
_publ_section_title
;
 Self-assembled multicomponent Pd6 aggregates showing low-humidity proton
 conduction
;
_journal_name_full               Chem.Commun.
_journal_page_first              1595
_journal_paper_doi               10.1039/c3cc47965j
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C104 H148 N32 Pd6, 12(N O3), 41(H2O)'
_chemical_formula_sum            'C104 H230 N44 O77 Pd6'
_chemical_formula_weight         3967.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 127.435(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.0277(19)
_cell_length_b                   11.5534(5)
_cell_length_c                   35.1453(14)
_cell_measurement_reflns_used    14208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.0
_cell_volume                     16129.9(12)
_computing_cell_refinement       'Bruker saint'
_computing_data_collection       'Bruker kappa Apex-II ccd'
_computing_data_reduction        'Bruker saint'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  WinGXv1.80.05
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXL-2013
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.973
_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  0.1156
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            123439
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.025
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             8253.0
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
12(N O3), 41(H2O)  have been removed from formula unit 
by squeeze process.
;
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         14208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0797P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8341
_reflns_number_total             14208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc47965j.txt
_cod_data_source_block           Complex_2
_cod_database_code               7111858
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2013-4
_shelx_res_checksum              76644