Isolation and evolution of labile sulfur allotropesviakinetic encapsulation in interactive porous networks
Kitagawa, Hakuba; Ohtsu, Hiroyoshi; Cruz-Cabeza, Aurora J.; Kawano, Masaki; IUCrJ 3 (2016) –; doi:10.1107/S2052252516008423

data_1543412
_publ_section_title
;
 Isolation and evolution of labile sulfur allotropesviakinetic
 encapsulation in interactive porous networks
;
_journal_coeditor_code           ED5008
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252516008423
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         '(CuI)2 (N1C5H4C6H4)4C (S2)0.975'
_chemical_formula_sum            'C45 H32 Cu2 I2 N4 S1.95'
_chemical_formula_weight         1070.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2563(2)
_cell_length_b                   13.2563(2)
_cell_length_c                   27.5616(7)
_cell_measurement_reflns_used    20372
_cell_measurement_temperature    30(5)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.11
_cell_volume                     4843.39(16)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      30(5)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'KEK PF-AR NW2A beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68990
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            20372
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.9077
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 Scalepack'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.225
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.749
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                2025
_reflns_number_total             3092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ed5008.cif
_cod_data_source_block           S_dimer
_cod_original_cell_volume        4843.4(2)
_cod_database_code               1543412
_publcif_datablock.id            {74473b52-7f26-46c8-900c-9494eaec7b99}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes y