Order-disorder structural phase transition and magnetocaloric effect in organic-inorganic halide hybrid (C2H5NH3)2CoCl4
Sen, Abhijit; Roy, Soumyabrata; Peter, Sebastian C.; Paul, Arpita; Waghmare, Umesh V.; Sundaresan, A.; Journal of Solid State Chemistry 258 (2018) 431–440; doi:10.1016/j.jssc.2017.10.036

data_1561249
_publ_section_title
;
 Order-disorder structural phase transition and magnetocaloric effect in
 organic-inorganic halide hybrid (C2H5NH3)2CoCl4
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              431
_journal_page_last               440
_journal_paper_doi               10.1016/j.jssc.2017.10.036
_journal_volume                  258
_journal_year                    2018
_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           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6216(12)
_cell_length_b                   9.6734(15)
_cell_length_c                   16.831(3)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.305
_cell_measurement_theta_min      2.420
_cell_volume                     1240.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9301
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0895 before and 0.0674 after correction. The Ratio of minimum to maximum transmission is 0.6975. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Flack x determined using 1039 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.169(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0272P)^2^+1.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                2765
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            100K.cif
_cod_data_source_block           100K
_cod_original_cell_volume        1240.9(3)
_cod_database_code               1561249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
2.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C1(H1D,H1E,H1F)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              77936
_shelx_hkl_checksum              72209