Effect of the transition metal on the structure and order-disorder phase transition in layered hybrid metal halides (CH<sub>3</sub>CH<sub>2</sub>NH<sub>3</sub>)<sub>2</sub>[MCl<sub>4</sub>] (M = Mn and Co).
Jakhi, Shatakshi S.; Dhanetwal, Meenal; Reddy, V. Raghavendra; Hathwar, Venkatesha R.; Acta crystallographica Section B, Structural science, crystal engineering and materials 81 (2025) –; doi:10.1107/S2052520625002719

data_2312857
_publ_section_title
;
 Effect of the transition metal on the structure and order-disorder phase
 transition in layered hybrid metal halides
 (CH<sub>3</sub>CH<sub>2</sub>NH<sub>3</sub>)<sub>2</sub>[MCl<sub>4</sub>]
 (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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1098P)^2^+1.2926P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            woz5005sup1.cif
_cod_data_source_block           EACo_HT
_cod_database_code               2312857
_shelxl_version_number           2014-1
_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)
;
_shelx_res_checksum              62590
_shelx_hkl_checksum              13849
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2312857