Syntheses and investigation of metal complexes with macrocyclic polythioether ligands.
Rotärmel, Thomas; Becker, Jonathan; Schindler, Siegfried; Faraday discussions 234 (2022) 70–85; doi:10.1039/d1fd00062d

data_1564959
_publ_section_title
;
 Syntheses and investigation of metal complexes with macrocyclic
 polythioether ligands.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              70
_journal_page_last               85
_journal_paper_doi               10.1039/d1fd00062d
_journal_volume                  234
_journal_year                    2022
_chemical_formula_sum            'C28 H52 Fe3 I6 N4 S8'
_chemical_formula_weight         1630.16
_chemical_name_common            '[FeII(14-S~4~)(MeCN)2][(FeI3)2(14-S~4~)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2021-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.373(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8349(13)
_cell_length_b                   19.1835(12)
_cell_length_c                   15.1569(11)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.42
_cell_volume                     5083.9(6)
_computing_cell_refinement       'SAINT 8.40A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2019.1-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.40A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            124242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
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_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    4.842
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_exptl_absorpt_correction_T_min  0.4755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2(Sheldrick, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.203
_refine_diff_density_max         2.898
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         13139
_refine_ls_number_restraints     830
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0581
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_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^)+(0.0368P)^2^+27.7739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10253
_reflns_number_total             13139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00062d2.cif
_cod_data_source_block           D20321
_cod_depositor_comments
'Adding full bibliography for 1564950--1564960.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.225
_shelx_estimated_absorpt_t_max   0.440
_shelx_res_checksum              91952