A single H-bond triggers the formation of a cleft around Et<sub>3</sub>NH<sup>+</sup> through bond rearrangement and rotations of arms in both Co(III) and Fe(III) complexes.
Paik, Somnath; Ray, Manabendra; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17448–17451; doi:10.1039/d4dt02515f

data_7717205
_publ_section_title
;
 A single H-bond triggers the formation of a cleft around
 Et<sub>3</sub>NH<sup>+</sup> through bond rearrangement and rotations of
 arms in both Co(III) and Fe(III) complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17448
_journal_page_last               17451
_journal_paper_doi               10.1039/d4dt02515f
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C38 H36 Fe N4 O8, C6 H16 N, C6 H13 N, Cl O4'
_chemical_formula_sum            'C50 H65 Cl Fe N6 O12'
_chemical_formula_weight         1033.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-27 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.402(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7580(10)
_cell_length_b                   19.6919(19)
_cell_length_c                   27.323(3)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.20
_cell_volume                     5241.0(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            110437
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.068
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       Block
_exptl_crystal_F_000             2184
_exptl_crystal_recrystallization_method ' Methanol DMF Slow evaporation'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.5760
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3970 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.124(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1275
_refine_ls_number_reflns         18351
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+8.8023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                11787
_reflns_number_total             18351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02515f2.cif
_cod_data_source_block           Complex_5
_cod_depositor_comments
'Adding full bibliography for 7717202--7717205.cif.'
_cod_original_cell_volume        5240.9(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7717205
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              44311
_shelx_hkl_checksum              97941