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_1556689
_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            'C22 H40 I16 N8'
_chemical_formula_weight         2447.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                108.167(4)
_cell_angle_beta                 94.071(5)
_cell_angle_gamma                104.453(4)
_cell_formula_units_Z            2
_cell_length_a                   8.300(1)
_cell_length_b                   16.191(2)
_cell_length_c                   21.221(3)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      2.54
_cell_volume                     2589.3(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59174
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    9.586
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.3769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    3.138
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.422
_refine_diff_density_min         -4.595
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9410
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0619P)^2^+27.2314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8865
_reflns_number_total             9410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-48.cif
_cod_data_source_block           1
_cod_original_cell_volume        2589.5(6)
_cod_database_code               1556689
_shelx_estimated_absorpt_t_min   0.161
_shelx_estimated_absorpt_t_max   0.597
_shelx_res_checksum              8177
_shelx_hkl_checksum              84193