An I 6 2 − ${μathrm{I}}_{6}^{2-}$ anion in the crystal structure of theophyllinium triiodide monohydrate, C7H11I3N4O3
Reiss, Guido J.; Wyshusek, Maik; Rheinländer, Jana C.; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1017–1020; doi:10.1515/ncrs-2022-0358

data_8107280
_publ_section_title
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 An I 6 2 &#x2212; ${\mathrm{I}}_{6}^{2-}$ anion in the crystal structure
 of theophyllinium triiodide monohydrate, C7H11I3N4O3
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1017
_journal_page_last               1020
_journal_paper_doi               10.1515/ncrs-2022-0358
_journal_volume                  237
_journal_year                    2022
_chemical_formula_sum            'C7 H11 I3 N4 O3'
_chemical_formula_weight         579.90
_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                76.2062(14)
_cell_angle_beta                 88.2421(13)
_cell_angle_gamma                89.4102(13)
_cell_formula_units_Z            4
_cell_length_a                   9.28478(14)
_cell_length_b                   12.2214(2)
_cell_length_c                   13.4088(2)
_cell_measurement_reflns_used    45745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8800
_cell_measurement_theta_min      2.1980
_cell_volume                     1476.95(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Diamond 4.5.2 (Crystal Impact, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64027
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         4.082
_diffrn_source                   'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.352
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.262
_refine_diff_density_min         -1.748
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         10661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+2.000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0493
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9468
_reflns_number_total             10661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0358_suppl.cif
_cod_data_source_block           Theowhat_I8_auto_a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
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_cod_database_code               8107280
_shelx_res_checksum              59550
_shelx_hkl_checksum              57670