Mechanism of Pressure-Induced Phase Transitions and Structure‒Property Relations in Methylhydrazinium Manganese Hypophosphite Perovskites
Mączka, Mirosław; Sobczak, Szymon; Kryś, Mikołaj; Leite, Fabio Furtado; Paraguassu, Waldeci; Katrusiak, Andrzej; The Journal of Physical Chemistry C  (2021) –; doi:10.1021/acs.jpcc.1c01998

data_1562294
_publ_section_title
;
 Mechanism of Pressure-Induced Phase Transitions and Structure--Property
 Relations in Methylhydrazinium Manganese Hypophosphite Perovskites
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.1c01998
_journal_year                    2021
_chemical_formula_moiety         'H6 Mn O6 P3, C H7 N2'
_chemical_formula_sum            'C H13 Mn N2 O6 P3'
_chemical_formula_weight         297.99
_chemical_name_common            HMyMnPO2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-02-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-02-25 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.533(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2348(11)
_cell_length_b                   7.272(2)
_cell_length_c                   12.6997(8)
_cell_measurement_reflns_used    2276
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6120
_cell_measurement_theta_min      4.6190
_cell_volume                     944.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1370000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.478
_diffrn_measured_fraction_theta_max 0.362
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  19.75   0.75   32.00   0.00 -30.00   0.00    --    73
  2  \f    140.00 200.00   0.75   32.00   0.00 -30.00   0.00    --    80
  3  \f    160.00 217.00   0.75   32.00   0.00  30.00   0.00    --    76
  4  \f    -20.00  34.75   0.75   32.00   0.00  30.00   0.00    --    73
  5  \w    -24.00  24.00   0.75   32.00    --   30.00  39.46 -12.90   64
  6  \w    -24.00  24.00   0.75   32.00    --   30.00  39.46 167.10   64
  7  \w    -50.00  10.00   0.75   32.00    --  -30.00  39.46 167.10   80
  8  \w    -50.00  10.00   0.75   32.00    --  -30.00  39.46 -12.90   80
  9  \w    -64.00  -8.50   0.75   32.00    --  -30.00  81.40 -28.90   74
 10  \w    -64.00  -8.50   0.75   32.00    --  -30.00  81.40 151.10   74
 11  \w    -19.00   8.00   0.75   32.00    --   30.00  81.40 151.10   36
 12  \w    -19.00   8.00   0.75   32.00    --   30.00  81.40 -28.90   36
 13  \w    -43.00 -21.25   0.75   32.00    --   30.00 134.60 -56.90   29
 14  \w    -43.00 -21.25   0.75   32.00    --   30.00 134.60 123.10   29
 15  \w    -90.00 -36.00   0.75   32.00    --  -30.00 134.60 123.10   72
 16  \w    -90.00 -36.00   0.75   32.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.478
_diffrn_reflns_Laue_measured_fraction_max 0.362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3855
_diffrn_reflns_point_group_measured_fraction_full 0.478
_diffrn_reflns_point_group_measured_fraction_max 0.362
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.784
_diffrn_reflns_theta_min         4.646
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0554P)^2^+4.1640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                564
_reflns_number_total             729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c01998_si_002.cif
_cod_data_source_block           mhymnpo2_1_37
_cod_database_code               1562294
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Sof: Mn2(0.5) Mn1(0.5)
 Fixed Uiso: H1(0.027) H2(0.027) H3(0.028) H4(0.028) H6(0.027) H5(0.027)
 H13(0.044) H14(0.044) H15(0.044) H12(0.054) H11(0.054) H16(0.04) H10(0.04)
 Fixed X: Mn2(0.5) Mn1(0) H1(0.17847) H2(0.133884) H3(0.199802) H4(0.165276)
 H6(0.613092) H5(0.683201) H13(0.456954) H14(0.477645) H15(0.550683)
 H12(0.361643) H11(0.369531) H16(0.239711) H10(0.219039)
 Fixed Y: Mn2(1) Mn1(0.5) H1(0.482378) H2(0.301738) H3(0.828188) H4(0.997401)
 H6(0.570667) H5(0.516558) H13(0.471816) H14(0.54773) H15(0.639076)
 H12(0.788148) H11(0.742054) H16(0.519377) H10(0.586981)
 Fixed Z: Mn2(0.5) Mn1(0.5) H1(0.231219) H2(0.285232) H3(0.422522)
 H4(0.491914) H6(0.457365) H5(0.564423) H13(0.724278) H14(0.839342)
 H15(0.746845) H12(0.79708) H11(0.683239) H16(0.712629) H10(0.814248)
;
_shelx_res_checksum              47953
_shelx_hkl_checksum              95829
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;