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_1543414
_publ_section_title
;
 Isolation and evolution of labile sulfur allotropesviakinetic
 encapsulation in interactive porous networks
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252516008423
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety
'(CuI)1.88 (N1C5H4C6H4)4C (cycro-S3)0.62 (bent-S3)0.39'
_chemical_formula_sum            'C45 H32 Cu1.88 I1.88 N4 S3.01'
_chemical_formula_weight         1083.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8758(4)
_cell_length_b                   26.8758(4)
_cell_length_c                   7.1689(1)
_cell_measurement_reflns_used    52191
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.077
_cell_measurement_theta_min      2.698
_cell_volume                     5178.16(13)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            52191
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         28.077
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.6195
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2141
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1625 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.430(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     397
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.1257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3852
_reflns_number_total             4353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed5008.cif
_cod_data_source_block           300K_S_helical
_cod_original_cell_volume        5178.1(2)
_cod_database_code               1543414
_shelx_estimated_absorpt_t_min   0.232
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2014-3
_shelx_res_checksum              88650
_shelx_hkl_checksum              39264