Exact mass analysis of sulfur clusters upon encapsulation by a polyaromatic capsular matrix
Sho Matsuno; Masahiro Yamashina; Yoshihisa Sei; Munetaka Akita; Akiyoshi Kuzume; Kimihisa Yamamoto; Michito Yoshizawa; Nature Communications 8 (2017) 749–; doi:10.1038/s41467-017-00605-5

data_1547694
_publ_section_title
;
 Exact mass analysis of sulfur clusters upon encapsulation by a
 polyaromatic capsular matrix
;
_journal_name_full               'Nature Communications'
_journal_page_first              749
_journal_paper_doi               10.1038/s41467-017-00605-5
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C212 H184 N12 O46 Pd2 S12'
_chemical_formula_weight         4233.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                70.0170(10)
_cell_angle_beta                 69.0620(10)
_cell_angle_gamma                61.4680(10)
_cell_formula_units_Z            2
_cell_length_a                   21.297(2)
_cell_length_b                   21.480(2)
_cell_length_c                   27.276(3)
_cell_measurement_reflns_used    7400
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.3845
_cell_measurement_theta_min      2.207
_cell_volume                     10013.5(17)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.1536
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38446
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        22.464
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_min         1.221
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       prism
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.813
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2765
_refine_ls_number_reflns         25841
_refine_ls_number_restraints     4572
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.1346
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^+0.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3689
_refine_ls_wR_factor_ref         0.4282
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14302
_reflns_number_total             25841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41467_2017_605_MOESM4_ESM.cif
_cod_data_source_block           SM321
_cod_original_cell_volume        10013.2(17)
_cod_database_code               1547694
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              79341
_shelx_hkl_checksum              87547