Crystal structure of caffeinium triiodide – caffeine (1/1), C16H21I3N8O4
Merkelbach, Johannes; Majewski, Martha A.; Reiss, Guido J.; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 941–944; doi:10.1515/ncrs-2018-0125

data_8106355
_publ_section_title
;
 Crystal structure of caffeinium triiodide -- caffeine (1/1), C16H21I3N8O4
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              941
_journal_page_last               944
_journal_paper_doi               10.1515/ncrs-2018-0125
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C8 H11 N4 O2, C8 H10 N4 O2, I3'
_chemical_formula_sum            'C16 H21 I3 N8 O4'
_chemical_formula_weight         770.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 114.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7257(7)
_cell_length_b                   10.5712(5)
_cell_length_c                   16.7501(8)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      31.83
_cell_measurement_theta_min      2.34
_cell_volume                     2374.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 4.5.1 (Brandenburg, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50390
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        28.497
_diffrn_reflns_theta_max         28.497
_diffrn_reflns_theta_min         1.553
_exptl_absorpt_coefficient_mu    3.988
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
No additional spherical absorption correction. 
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.00069(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5051
_reflns_number_total             6007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0125_suppl.cif
_cod_data_source_block           7_runs
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8106355
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.715
_shelx_res_checksum              34410
_shelx_hkl_checksum              29110