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_1547693
_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 H181 N8 O34 Pd2 S16'
_chemical_formula_weight         4110.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.856(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7593(11)
_cell_length_b                   33.6872(16)
_cell_length_c                   28.3246(14)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    273
_cell_measurement_theta_max      66.7201
_cell_measurement_theta_min      2.824
_cell_volume                     20736.4(18)
_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      273
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1531
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            151419
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.501
_exptl_absorpt_coefficient_mu    3.488
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             8516
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.141
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2449
_refine_ls_number_reflns         36442
_refine_ls_number_restraints     3712
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.1955
_refine_ls_R_factor_gt           0.1355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3575
_refine_ls_wR_factor_ref         0.4022
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                21447
_reflns_number_total             36442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41467_2017_605_MOESM3_ESM.cif
_cod_data_source_block           SM253
_cod_database_code               1547693
_shelx_estimated_absorpt_t_min   0.660
_shelx_estimated_absorpt_t_max   0.700
_shelx_res_checksum              3620
_shelx_hkl_checksum              86073
_shelx_fab_checksum              9053