Synthesis and crystal structure study of (<i>R</i>,<i>R</i>)-TMCDA ethanol derivatives doubly protonated with FeCl<sub>4</sub> <sup>-</sup> and Cl<sup>-</sup> as counter-ions.
Klotz, Franziska Dorothea; Alonso Felipe, Clara; Villafañe, Fernando; Strohmann, Carsten; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 372–376; doi:10.1107/S2056989025003019

data_2023463
_publ_section_title
;
 Synthesis and crystal structure study of (<i>R</i>,<i>R</i>)-TMCDA
 ethanol derivatives doubly protonated with FeCl<sub>4</sub> <sup>-</sup>
 and Cl<sup>-</sup> as counter-ions.
;
_journal_coeditor_code           ZN2042
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              372
_journal_page_last               376
_journal_paper_doi               10.1107/S2056989025003019
_journal_volume                  81
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_iupac          '(C11 H26 N2 O) [Fe Cl4] Cl'
_chemical_formula_moiety         'C11 H26 N2 O 2+, Cl4 Fe -, Cl -'
_chemical_formula_sum            'C11 H26 Cl5 Fe N2 O'
_chemical_formula_weight         435.44
_chemical_name_systematic
'(<i>R</i>,<i>R</i>)-<i>N</i>^1^-(2-Hydroxyethyl)-<i>N</i>^1^,<i>N</i>^2^,<i>N</i>^2^-trimethylcyclohexane-1,2-bis(aminium) tetrachloridoferrate chloride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6070(5)
_cell_length_b                   11.5870(6)
_cell_length_c                   21.8705(13)
_cell_measurement_reflns_used    9581
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      34.786
_cell_measurement_theta_min      2.562
_cell_volume                     1927.7(2)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2016)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL  (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i>  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            144077
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.999
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_T_max  0.5668
_exptl_absorpt_correction_T_min  0.4716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       needle
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.480
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3373 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.013(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         8488
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.5573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                8082
_reflns_number_total             8488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zn2042.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 2023463--2023464.cif.'
_cod_database_code               2023463
_shelx_estimated_absorpt_t_min   0.386
_shelx_estimated_absorpt_t_max   0.783
_shelx_hkl_checksum              44263
_shelx_res_checksum              78690