Unprecedented transformation of [I(-)·I3(-)] to [I4(2-)] polyiodides in the solid state: structures, phase transitions and characterization of dipyrazolium iodide triiodide.
Węcławik, M; Szklarz, P.; Medycki, W.; Janicki, R.; Piecha-Bisiorek, A; Zieliński, P; Jakubas, R.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18447–18458; doi:10.1039/c5dt02265g

data_7036638
_publ_section_title
;
 Unprecedented transformation of [I(-)&#x00B7;I3(-)] to [I4(2-)]
 polyiodides in the solid state: structures, phase transitions and
 characterization of dipyrazolium iodide triiodide.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18447
_journal_page_last               18458
_journal_paper_doi               10.1039/c5dt02265g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C6 H10 I4 N4'
_chemical_formula_sum            'C6 H10 I4 N4'
_chemical_formula_weight         645.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-09-01 deposited with the CCDC.
2015-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.162(6)
_cell_length_b                   7.913(3)
_cell_length_c                   13.627(4)
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      36.6616
_cell_measurement_theta_min      2.8700
_cell_volume                     1527.1(10)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         36.760
_diffrn_reflns_theta_min         2.877
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.139
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.809
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.2767
_exptl_crystal_size_mid          0.1722
_exptl_crystal_size_min          0.0963
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+1.7745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1034
_reflns_number_total             1847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02265g2.cif
_cod_data_source_block           295k
_cod_depositor_comments
'Adding full bibliography for 7036637--7036638.cif.'
_cod_database_code               7036638
_shelxl_version_number           2013-4
_shelx_res_checksum              51316