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_1543416
_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)1.85 (N1C5H4C6H4)4C (S2)1.50'
_chemical_formula_sum            'C45 H32 Cu1.85 I1.85 N4 S3'
_chemical_formula_weight         1077.31
_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                   26.8664(4)
_cell_length_b                   26.8664(4)
_cell_length_c                   7.1717(1)
_cell_measurement_reflns_used    65225
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      29.511
_cell_measurement_theta_min      2.361
_cell_volume                     5176.56(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 0.997
_diffrn_measured_fraction_theta_max 0.833
_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     0.700
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            65225
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.511
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.861
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2129
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.155(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6115
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0755P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                4784
_reflns_number_total             6115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed5008.cif
_cod_data_source_block           300k_only_once
_cod_original_cell_volume        5176.5(2)
_cod_database_code               1543416
_shelx_estimated_absorpt_t_min   0.332
_shelx_estimated_absorpt_t_max   0.913
_shelxl_version_number           2014-3
_shelx_res_checksum              64097
_shelx_hkl_checksum              11245