#------------------------------------------------------------------------------
#$Date: 2025-05-29 05:16:57 +0300 (Thu, 29 May 2025) $
#$Revision: 299862 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/28/2312855.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312855
loop_
_publ_author_name
'Jakhi, Shatakshi S.'
'Dhanetwal, Meenal'
'Reddy, V. Raghavendra'
'Hathwar, Venkatesha R.'
_publ_section_title
;
 Effect of the transition metal on the structure and order-disorder phase
 transition in layered hybrid metal halides
 (CH₃CH₂NH₃)₂[MCl₄]
 (M = Mn and Co).
;
_journal_issue                   3
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520625002719
_journal_volume                  81
_journal_year                    2025
_chemical_formula_moiety         'Cl4 Mn, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Cl4 Mn N2'
_chemical_formula_weight         288.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1748(5)
_cell_length_b                   5.1748(5)
_cell_length_c                   22.112(3)
_cell_measurement_reflns_used    1456
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      3.686
_cell_volume                     592.13(11)
_computing_cell_refinement       'SAINT (Bruker, 2022)'
_computing_data_collection       'SAINT (Bruker, 2022)'
_computing_data_reduction        'SAINT (Bruker, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3486
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         3.686
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0365
_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/[σ²(Fo²)+(0.0314P)²+2.2579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                259
_reflns_number_total             259
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            woz5005sup1.cif
_cod_data_source_block           EAMn_HT
_cod_original_cell_volume        592.12(14)
_cod_database_code               2312855
_shelxl_version_number           2014-1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1(0.125) C2(0.125) H1(0.125) H1A(0.125)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.5000 0.5000 0.0242(4) Uani 1 16 d S T P . .
Cl1 Cl 0.5000 0.0000 0.5000 0.0580(7) Uani 1 8 d S T P . .
Cl2 Cl 0.5000 0.5000 0.38897(9) 0.0837(10) Uani 1 8 d S T P . .
N1 N 0.0000 0.0000 0.3985(3) 0.0491(18) Uani 1 8 d S T P . .
C1 C 0.0000 0.091(3) 0.3371(8) 0.059(6) Uani 0.25 2 d S T P . .
C2 C 0.0000 -0.109(5) 0.2904(6) 0.083(11) Uani 0.25 2 d S T P . .
H2 H 0.0000 0.0000 0.262(6) 0.08(4) Uiso 1 8 d S . P . .
H1 H 0.097(14) 0.097(14) 0.411(5) 0.00(3) Uiso 0.25 2 d S . P . .
H1A H 0.08(3) 0.23(3) 0.338(6) 0.00(3) Uiso 0.125 1 d . . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Mn1 Cl1 180.0 . 1_565 ?
Cl1 Mn1 Cl1 180.0 3 3_655 ?
Cl1 Mn1 Cl1 90.0 1_565 3_655 ?
Cl1 Mn1 Cl1 90.0 . 3 ?
Cl1 Mn1 Cl1 90.0 1_565 3 ?
Cl1 Mn1 Cl1 90.0 . 3_655 ?
Cl2 Mn1 Cl1 90.0 . 3 ?
Cl2 Mn1 Cl1 90.0 17_666 3_655 ?
Cl2 Mn1 Cl1 90.0 17_666 1_565 ?
Cl2 Mn1 Cl1 90.0 17_666 3 ?
Cl2 Mn1 Cl1 90.0 . 1_565 ?
Cl2 Mn1 Cl1 90.0 . . ?
Cl2 Mn1 Cl1 90.0 17_666 . ?
Cl2 Mn1 Cl1 90.0 . 3_655 ?
Cl2 Mn1 Cl2 180.0 . 17_666 ?
Mn1 Cl1 Mn1 180.0 1_545 . ?
C1 N1 C1 26.9(10) 3 2 ?
C1 N1 C1 26.9(10) 4 . ?
C1 N1 C1 26.9(10) 3 . ?
C1 N1 C1 38.4(15) 3 4 ?
C1 N1 C1 26.9(10) 2 4 ?
C1 N1 C1 38.4(15) 2 . ?
C1 N1 H1 124(8) 3 . ?
C1 N1 H1 98(8) 4 . ?
C1 N1 H1 124(8) 2 . ?
C1 N1 H1 98(8) . . ?
N1 C1 C2 115.8(15) . . ?
N1 C1 H1A 105(9) . . ?
C1 C1 N1 70.8(7) 2 . ?
C1 C1 N1 76.6(5) 4 . ?
C1 C1 N1 76.6(5) 3 . ?
C1 C1 C1 90.002(13) 3 4 ?
C1 C1 C1 45.001(7) 3 2 ?
C1 C1 C1 45.001(10) 4 2 ?
C1 C1 C2 68.1(8) 2 4 ?
C1 C1 C2 60.0(6) 3 . ?
C1 C1 C2 93.5(13) 4 2 ?
C1 C1 C2 92.9(10) 3 3 ?
C1 C1 C2 93.5(13) 3 2 ?
C1 C1 C2 54.7(10) 4 3 ?
C1 C1 C2 92.9(10) 4 4 ?
C1 C1 C2 68.1(8) 2 3 ?
C1 C1 C2 45.0(11) 2 . ?
C1 C1 C2 95.0(18) 2 2 ?
C1 C1 C2 54.7(10) 3 4 ?
C1 C1 C2 60.0(6) 4 . ?
C1 C1 H1A 149(8) 2 . ?
C1 C1 H1A 104(9) 4 . ?
C1 C1 H1A 166(8) 3 . ?
C2 C1 N1 130.3(13) 4 . ?
C2 C1 N1 130.3(13) 3 . ?
C2 C1 N1 166(2) 2 . ?
C2 C1 C2 32.9(14) 3 . ?
C2 C1 C2 32.9(14) 4 . ?
C2 C1 C2 38.8(19) 2 4 ?
C2 C1 C2 38.8(19) 2 3 ?
C2 C1 C2 53(2) 4 3 ?
C2 C1 C2 50(2) 2 . ?
C2 C1 H1A 96(9) 3 . ?
C2 C1 H1A 124(10) 4 . ?
C2 C1 H1A 128(9) . . ?
C2 C1 H1A 87(9) 2 . ?
C1 C2 C1 27.2(10) 3 . ?
C1 C2 C1 40.1(17) 2 . ?
C1 C2 C1 27.2(10) 4 . ?
C1 C2 C1 43.8(17) 4 3 ?
C1 C2 C1 31.7(13) 2 3 ?
C1 C2 C1 31.7(13) 2 4 ?
C1 C2 C2 85.0(18) 2 2 ?
C1 C2 H2 109(6) 3 . ?
C1 C2 H2 94(7) . . ?
C1 C2 H2 134(7) 2 . ?
C1 C2 H2 109(6) 4 . ?
C2 C2 C1 54.7(10) 4 3 ?
C2 C2 C1 63.7(12) 2 4 ?
C2 C2 C1 45.0(11) 2 . ?
C2 C2 C1 87.1(10) 4 4 ?
C2 C2 C1 86.5(13) 4 2 ?
C2 C2 C1 54.7(10) 3 4 ?
C2 C2 C1 87.1(10) 3 3 ?
C2 C2 C1 60.0(6) 3 . ?
C2 C2 C1 63.7(12) 2 3 ?
C2 C2 C1 86.5(13) 3 2 ?
C2 C2 C1 60.0(6) 4 . ?
C2 C2 C2 89.998(11) 3 4 ?
C2 C2 C2 44.999(7) 4 2 ?
C2 C2 C2 44.999(7) 3 2 ?
C2 C2 H2 62(4) 4 . ?
C2 C2 H2 62(4) 3 . ?
C2 C2 H2 49(6) 2 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 Cl1 2.5874(3) 3_655 ?
Mn1 Cl1 2.5874(3) 3 ?
Mn1 Cl1 2.5874(3) 1_565 ?
Mn1 Cl1 2.5874(3) . ?
Mn1 Cl2 2.455(2) . ?
Mn1 Cl2 2.455(2) 17_666 ?
Cl1 Mn1 2.5874(3) 1_545 ?
N1 C1 1.438(18) 3 ?
N1 C1 1.438(18) 4 ?
N1 C1 1.438(18) 2 ?
N1 C1 1.438(18) . ?
N1 H1 0.76(10) . ?
C1 C1 0.94(4) 2 ?
C1 C1 0.67(3) 3 ?
C1 C1 0.67(3) 4 ?
C1 C2 1.04(2) 2 ?
C1 C2 1.27(2) 3 ?
C1 C2 1.46(3) . ?
C1 C2 1.27(2) 4 ?
C1 H1A 0.86(15) . ?
C2 C1 1.27(2) 4 ?
C2 C1 1.27(2) 3 ?
C2 C1 1.04(2) 2 ?
C2 C2 0.80(4) 4 ?
C2 C2 1.12(5) 2 ?
C2 C2 0.80(4) 3 ?
C2 H2 0.85(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C1 54.8(5) . . . 3 ?
N1 C1 C2 C1 -54.8(5) . . . 4 ?
N1 C1 C2 C1 0.000(6) . . . 2 ?
N1 C1 C2 C2 125.2(5) . . . 4 ?
N1 C1 C2 C2 -125.2(5) . . . 3 ?
N1 C1 C2 C2 180.000(5) . . . 2 ?
C1 N1 C1 C1 46.64(13) 2 . . 3 ?
C1 N1 C1 C1 -46.64(12) 3 . . 2 ?
C1 N1 C1 C1 -46.64(13) 2 . . 4 ?
C1 N1 C1 C1 93.3(3) 4 . . 3 ?
C1 N1 C1 C1 46.64(13) 4 . . 2 ?
C1 N1 C1 C1 -93.3(3) 3 . . 4 ?
C1 N1 C1 C2 46.64(12) 4 . . . ?
C1 N1 C1 C2 -46.64(13) 3 . . . ?
C1 N1 C1 C2 0.00(3) 2 . . 2 ?
C1 N1 C1 C2 -46.64(12) 3 . . 2 ?
C1 N1 C1 C2 -35.6(17) 2 . . 3 ?
C1 N1 C1 C2 46.64(13) 4 . . 2 ?
C1 N1 C1 C2 11.0(18) 4 . . 3 ?
C1 N1 C1 C2 35.6(17) 2 . . 4 ?
C1 N1 C1 C2 0.000(5) 2 . . . ?
C1 N1 C1 C2 82.2(16) 4 . . 4 ?
C1 N1 C1 C2 -82.2(16) 3 . . 3 ?
C1 N1 C1 C2 -11.0(18) 3 . . 4 ?
C1 C1 C2 C1 -54.8(5) 3 . . 2 ?
C1 C1 C2 C1 -54.8(5) 2 . . 4 ?
C1 C1 C2 C1 109.5(10) 4 . . 3 ?
C1 C1 C2 C1 54.8(5) 4 . . 2 ?
C1 C1 C2 C1 54.8(5) 2 . . 3 ?
C1 C1 C2 C1 -109.5(11) 3 . . 4 ?
C1 C1 C2 C2 180.002(14) 4 . . 4 ?
C1 C1 C2 C2 -125.2(5) 2 . . 3 ?
C1 C1 C2 C2 125.2(5) 3 . . 2 ?
C1 C1 C2 C2 180.000(11) 2 . . 2 ?
C1 C1 C2 C2 70.5(11) 3 . . 4 ?
C1 C1 C2 C2 179.998(4) 3 . . 3 ?
C1 C1 C2 C2 -70.5(10) 4 . . 3 ?
C1 C1 C2 C2 -125.2(5) 4 . . 2 ?
C1 C1 C2 C2 125.2(5) 2 . . 4 ?
C2 C1 C2 C1 180.000(13) 2 . . 2 ?
C2 C1 C2 C1 179.998(5) 4 . . 4 ?
C2 C1 C2 C1 -70.5(10) 4 . . 3 ?
C2 C1 C2 C1 -125.2(5) 4 . . 2 ?
C2 C1 C2 C1 -125.2(5) 2 . . 3 ?
C2 C1 C2 C1 125.2(5) 3 . . 2 ?
C2 C1 C2 C1 180.002(4) 3 . . 3 ?
C2 C1 C2 C1 125.2(5) 2 . . 4 ?
C2 C1 C2 C1 70.5(10) 3 . . 4 ?
C2 C1 C2 C2 54.8(5) 2 . . 3 ?
C2 C1 C2 C2 -54.8(5) 2 . . 4 ?
C2 C1 C2 C2 54.8(5) 4 . . 2 ?
C2 C1 C2 C2 109.5(10) 4 . . 3 ?
C2 C1 C2 C2 -109.5(11) 3 . . 4 ?
C2 C1 C2 C2 -54.8(5) 3 . . 2 ?

_cod_database_fobs_code 2312855
