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_1543413
_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 (S2)0.63 (S3)0.58'
_chemical_formula_sum            'C45 H32 Cu1.88 I1.88 N4 S3'
_chemical_formula_weight         1083.02
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -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                   26.7176(5)
_cell_length_b                   26.7176(5)
_cell_length_c                   7.1942(2)
_cell_measurement_reflns_used    91118
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.386
_cell_measurement_theta_min      2.714
_cell_volume                     5135.4(2)
_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      250(2)
_diffrn_measured_fraction_theta_full 0.778
_diffrn_measured_fraction_theta_max 0.977
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.778
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            91118
_diffrn_reflns_point_group_measured_fraction_full 0.772
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.714
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.707
_exptl_absorpt_correction_T_max  0.6691
_exptl_absorpt_correction_T_min  0.6198
_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    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2133
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1921 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.051(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     1237
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1773P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2346
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.766
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                4892
_reflns_number_total             7133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed5008.cif
_cod_data_source_block           250K_S_helical_initial
_cod_original_formula_sum        'C45 H32 Cu1.88 I1.88 N4 S3.00'
_cod_database_code               1543413
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2014-3
_shelx_res_checksum              78215
_shelx_hkl_checksum              62596