Cones with a three-fold symmetry constructed from three hydrogen bonded theophyllinium cations that coat [FeCl4]− anions in the crystal structure of tris(theophyllinium) bis(tetrachloridoferrate(III)) chloride trihydrate, C21H33Cl9Fe2N12O9
Reiss, Guido J.; Wyshusek, Maik; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 121–124; doi:10.1515/ncrs-2021-0399

data_8104977
_publ_section_title
;
 Cones with a three-fold symmetry constructed from three hydrogen bonded
 theophyllinium cations that coat [FeCl4]&#x2212; anions in the crystal
 structure of tris(theophyllinium) bis(tetrachloridoferrate(III)) chloride
 trihydrate, C21H33Cl9Fe2N12O9
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              121
_journal_page_last               124
_journal_paper_doi               10.1515/ncrs-2021-0399
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         '3(C7 H9 N4 O2), 2(Cl4 Fe), Cl, 3(H2 O)'
_chemical_formula_sum            'C21 H33 Cl9 Fe2 N12 O9'
_chemical_formula_weight         1028.34
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.1897(3)
_cell_length_b                   13.1897(3)
_cell_length_c                   39.5222(9)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.4720
_cell_measurement_theta_min      3.6970
_cell_volume                     5954.4(2)
_computing_cell_refinement       'Crysalis-Pro, RIGAKU 2020'
_computing_data_collection       'Crysalis-Pro, RIGAKU 2020'
_computing_data_reduction        'Crysalis-Pro, RIGAKU 2020'
_computing_molecular_graphics    'DIAMOND 4, CRYSTAL IMPACT 2020'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            20742
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        29.492
_diffrn_reflns_theta_max         29.492
_diffrn_reflns_theta_min         5.154
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       Block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0330P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3238
_reflns_number_total             3677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0399_suppl.cif
_cod_data_source_block           exp_1468_120_a
_cod_original_cell_volume        5954.4(3)
_cod_database_code               8104977
_shelx_res_checksum              27929