#------------------------------------------------------------------------------
#$Date: 2025-05-29 05:16:57 +0300 (Thu, 29 May 2025) $
#$Revision: 299862 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/28/2312857.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_2312857
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 Co, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Cl4 Co N2'
_chemical_formula_weight         292.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-16
_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            4
_cell_length_a                   10.0173(5)
_cell_length_b                   7.4027(4)
_cell_length_c                   17.5837(8)
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.243
_cell_measurement_theta_min      3.083
_cell_volume                     1303.92(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12094
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         3.083
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.627
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1732
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0619
_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)+(0.1098P)²+1.2926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1199
_reflns_number_total             1732
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            woz5005sup1.cif
_cod_data_source_block           EACo_HT
_cod_database_code               2312857
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 C1-C2
 1.54 with sigma of 0.01
 C1-N1
 1.35 with sigma of 0.01
 C3-C4
 1.54 with sigma of 0.01
 C3-N2
 1.35 with sigma of 0.01
3. Rigid bond restraints
 Cl2, Cl2'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl2': within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(Cl2') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: Cl2(0.25) Cl2'(0.25) H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
 C2(0.5) C3(0.5) H3A(0.5) H3B(0.5)
6.a Riding coordinates:
 C1(H1D,H1E), C3(H3A,H3B)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-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
Co1 Co 0.77171(9) 0.7500 0.54093(5) 0.0677(4) Uani 1 2 d S T P . .
Cl1 Cl 0.9893(2) 0.7500 0.56926(13) 0.1121(9) Uani 1 2 d S T P A .
Cl2 Cl 0.7379(15) 0.7500 0.4153(9) 0.097(5) Uani 0.5 2 d S TU P A 1
Cl2' Cl 0.7462(12) 0.817(2) 0.4122(8) 0.068(2) Uani 0.25 1 d . U P A 2
Cl3 Cl 0.66928(17) 0.50209(17) 0.58768(10) 0.1031(6) Uani 1 1 d . . . . .
N1 N 1.0623(7) 0.7500 0.3842(3) 0.0928(19) Uani 1 2 d DS T P . .
H1A H 1.1158 0.6670 0.4044 0.139 Uiso 0.5 1 calc R U P . .
H1B H 0.9779 0.7247 0.3960 0.139 Uiso 0.5 1 calc R U P . .
H1C H 1.0836 0.8583 0.4025 0.139 Uiso 0.5 1 calc R U P . .
N2 N 0.3728(9) 0.7500 0.5693(4) 0.118(3) Uani 1 2 d DS T P . .
C1 C 1.0774(16) 0.7500 0.3046(5) 0.226(11) Uani 1 2 d DS T P . .
H1D H 1.0870 0.6255 0.2883 0.271 Uiso 0.5 1 d R U P . .
H1E H 1.1621 0.8097 0.2956 0.271 Uiso 0.5 1 d R U P . .
C2 C 0.9746(16) 0.830(2) 0.2556(7) 0.153(8) Uani 0.5 1 d D . P . .
C3 C 0.3322(16) 0.8349(19) 0.6315(7) 0.132(5) Uani 0.5 1 d D U P . .
H3A H 0.2530 0.9057 0.6207 0.158 Uiso 0.5 1 d R U P . .
H3B H 0.4029 0.9214 0.6412 0.158 Uiso 0.5 1 d R U P . .
C4 C 0.310(2) 0.7500 0.7080(7) 0.172(6) Uani 1 2 d DS T 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'
Co Co 0.3494 0.9721 '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 Co1 Cl2' 108.9(3) . 7_575 ?
Cl1 Co1 Cl2' 108.9(3) . . ?
Cl1 Co1 Cl3 111.22(6) . 7_575 ?
Cl1 Co1 Cl3 111.22(6) . . ?
Cl2 Co1 Cl1 111.6(4) . . ?
Cl2 Co1 Cl3 106.9(2) . . ?
Cl2 Co1 Cl3 106.9(2) . 7_575 ?
Cl2' Co1 Cl2' 24.6(8) . 7_575 ?
Cl3 Co1 Cl2' 118.5(4) 7_575 7_575 ?
Cl3 Co1 Cl2' 118.5(4) . . ?
Cl3 Co1 Cl2' 97.5(4) 7_575 . ?
Cl3 Co1 Cl2' 97.5(4) . 7_575 ?
Cl3 Co1 Cl3 108.76(9) 7_575 . ?
Cl2' Cl2' Co1 77.7(4) 7_575 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C3 N2 C3 56.6(13) . 7_575 ?
N1 C1 H1D 107.7 . . ?
N1 C1 H1E 104.8 . . ?
N1 C1 C2 120.5(10) . . ?
N1 C1 C2 120.5(10) . 7_575 ?
H1D C1 H1E 107.3 . . ?
C2 C1 H1D 60.8 7_575 . ?
C2 C1 H1D 106.3 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1E 134.6 7_575 . ?
C2 C1 C2 47.7(15) 7_575 . ?
C2 C2 C1 66.1(7) 7_575 . ?
N2 C3 H3A 110.2 . . ?
N2 C3 H3B 103.5 . . ?
N2 C3 C4 125.9(12) . . ?
C3 C3 N2 61.7(6) 7_575 . ?
C3 C3 H3A 122.7 7_575 . ?
C3 C3 H3B 131.3 7_575 . ?
C3 C3 C4 65.2(6) 7_575 . ?
H3A C3 H3B 106.0 . . ?
C4 C3 H3A 106.4 . . ?
C4 C3 H3B 103.0 . . ?
C3 C4 C3 49.5(11) 7_575 . ?
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
Co1 Cl1 2.236(2) . ?
Co1 Cl2 2.234(15) . ?
Co1 Cl2' 2.330(13) . ?
Co1 Cl2' 2.330(13) 7_575 ?
Co1 Cl3 2.2576(14) 7_575 ?
Co1 Cl3 2.2576(14) . ?
Cl2' Cl2' 0.99(3) 7_575 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.408(8) . ?
N2 C3 1.326(9) 7_575 ?
N2 C3 1.326(9) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.467(9) 7_575 ?
C1 C2 1.467(9) . ?
C2 C2 1.19(4) 7_575 ?
C3 C3 1.26(3) 7_575 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.501(9) . ?
C4 C3 1.501(9) 7_575 ?
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 C2 -105.1(9) . . . 7_575 ?
N2 C3 C4 C3 -12(2) . . . 7_575 ?
C3 N2 C3 C4 13(2) 7_575 . . . ?

_cod_database_fobs_code 2312857
