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_7717202
_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 Co N4 O8, C8 H20 N, 2(H2 O)'
_chemical_formula_sum            'C46 H60 Co N5 O10'
_chemical_formula_weight         901.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1822(4)
_cell_length_b                   12.1822(4)
_cell_length_c                   30.3583(16)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.36
_cell_volume                     4505.4(3)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            63748
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.144
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       diamond
_exptl_crystal_F_000             1912
_exptl_crystal_recrystallization_method 'Slow evaporation from DMF MeOH mixture'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.952
_exptl_transmission_factor_min   0.909
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1402 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0460P)^2^+1.5359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3619
_reflns_number_total             3974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02515f2.cif
_cod_data_source_block           Complex_1
_cod_depositor_comments
'Adding full bibliography for 7717202--7717205.cif.'
_cod_original_cell_volume        4505.4(4)
_cod_database_code               7717202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              85675
_shelx_hkl_checksum              19712