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_1562297
_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         296.98
_chemical_name_common            MHyMnPO2
_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             2021-02-21
_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                 93.298(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.115(2)
_cell_length_b                   7.088(6)
_cell_length_c                   12.613(2)
_cell_measurement_reflns_used    1093
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3050
_cell_measurement_theta_min      4.8340
_cell_volume                     902.8(8)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2920000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.538
_diffrn_measured_fraction_theta_max 0.417
_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  19.60   0.60   25.00   0.00 -30.00   0.00    --    91
  2  \f    140.00 200.00   0.60   25.00   0.00 -30.00   0.00    --   100
  3  \f    160.00 217.00   0.60   25.00   0.00  30.00   0.00    --    95
  4  \f    -20.00  34.60   0.60   25.00   0.00  30.00   0.00    --    91
  5  \w    -24.00  24.00   0.60   25.00    --   30.00  39.46 -12.90   80
  6  \w    -24.00  24.00   0.60   25.00    --   30.00  39.46 167.10   80
  7  \w    -50.00  10.00   0.60   25.00    --  -30.00  39.46 167.10  100
  8  \w    -50.00  10.00   0.60   25.00    --  -30.00  39.46 -12.90  100
  9  \w    -64.00  -8.20   0.60   25.00    --  -30.00  81.40 -28.90   93
 10  \w    -64.00  -8.20   0.60   25.00    --  -30.00  81.40 151.10   93
 11  \w    -19.00   8.00   0.60   25.00    --   30.00  81.40 151.10   45
 12  \w    -19.00   8.00   0.60   25.00    --   30.00  81.40 -28.90   45
 13  \w    -43.00 -21.40   0.60   25.00    --   30.00 134.60 -56.90   36
 14  \w    -43.00 -21.40   0.60   25.00    --   30.00 134.60 123.10   36
 15  \w    -90.00 -36.00   0.60   25.00    --  -30.00 134.60 123.10   90
 16  \w    -90.00 -36.00   0.60   25.00    --  -30.00 134.60 -56.90   90
;
_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  0.0872
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.538
_diffrn_reflns_Laue_measured_fraction_max 0.417
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4062
_diffrn_reflns_point_group_measured_fraction_full 0.538
_diffrn_reflns_point_group_measured_fraction_max 0.417
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.262
_diffrn_reflns_theta_min         4.856
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    2.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         766
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.1178
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3123
_refine_ls_wR_factor_ref         0.3710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                472
_reflns_number_total             766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c01998_si_002.cif
_cod_data_source_block           mhymnpo2_2_92
_cod_database_code               1562297
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All P(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O00B \\sim O007 \\sim H00C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O007) \\sim Ueq, Uanis(O00B) \\sim Ueq, Uanis(P0) \\sim Ueq, : with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(P0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O008) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 H0B, O006, P2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H00C, O007, O00B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P0, P1, H0A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00E, N10, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O008, P2, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00B, P0, O00A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Uiso: H16(0.027) H10(0.027)
 Fixed X: H16(0.24089) H10(0.209459)
 Fixed Y: H16(0.51141) H10(0.60613)
 Fixed Z: H16(0.723121) H10(0.81543)
5.a Secondary CH2 refined with riding coordinates:
 P2(H2A,H2B), P1(H1A,H1B), P0(H0A,H0B), N10(H10A,H10B)
5.b Idealised Me refined as rotating group:
 C00E(H00A,H00B,H00C)
;
_shelx_res_checksum              75061
_shelx_hkl_checksum              3819
_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
;