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_1562291
_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, 0.5(C2 H12 N4)'
_chemical_formula_sum            'C H13 Mn N2 O6 P3'
_chemical_formula_weight         295.98
_chemical_name_common            MHyMnPO2
_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             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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3794(10)
_cell_length_b                   13.2922(4)
_cell_length_c                   8.5672(7)
_cell_measurement_reflns_used    4739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5640
_cell_measurement_theta_min      4.4330
_cell_volume                     1068.10(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         110000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.550
_diffrn_measured_fraction_theta_max 0.431
_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   35.00   0.00 -30.00   0.00    --    73
  2  \f    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  \f    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  \f    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  \w    -90.00 -63.75   0.75   35.00    --  -30.00 134.60 123.10   35
;
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.550
_diffrn_reflns_Laue_measured_fraction_max 0.431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4739
_diffrn_reflns_point_group_measured_fraction_full 0.550
_diffrn_reflns_point_group_measured_fraction_max 0.431
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.816
_diffrn_reflns_theta_min         4.448
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0751P)^2^+1.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                452
_reflns_number_total             512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c01998_si_002.cif
_cod_data_source_block           mhymnpo2_0_11
_cod_original_cell_volume        1068.10(14)
_cod_database_code               1562291
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Sof: H2C(0.5) H2D(0.5) H1(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
2.a Rotating group:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 P1(H1A,H1B), P2(H2A,H2B), N2(H2C,H2D)
2.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_shelx_res_checksum              90721
_shelx_hkl_checksum              96675
_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
- B-factor correction
;