Stabilization of Supramolecular Networks of Polyiodides with Protonated Small Tetra-azacyclophanes
Savastano, M.; Martinez-Camarena, A.; Bazzicalupi, C.; Delgado-Pinar, E.; Llinares, J.M.; Mariani, P.; Verdejo, B.; Garcia-Espana, E.; Bianchi, A.; Inorganics 7 (2019) 48–; doi:10.3390/inorganics7040048

data_1556690
_publ_section_title
;
 Stabilization of Supramolecular Networks of Polyiodides with Protonated
 Small Tetra-azacyclophanes
;
_journal_name_full               Inorganics
_journal_page_first              48
_journal_paper_doi               10.3390/inorganics7040048
_journal_volume                  7
_journal_year                    2019
_chemical_formula_sum            'C14 H23 I14 N4 O'
_chemical_formula_weight         2039.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.226(1)
_cell_length_b                   13.060(1)
_cell_length_c                   17.377(2)
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.36
_cell_measurement_theta_min      2.28
_cell_volume                     2025.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3116
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.282
_exptl_absorpt_coefficient_mu    10.714
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS-2016/2'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    3.345
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.637
_refine_diff_density_min         -3.065
_refine_diff_density_rms         0.525
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1443P)^2^+31.8804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2353
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2244
_reflns_number_total             2810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-48.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1556690
_shelx_res_checksum              45291
_shelx_hkl_checksum              22770