High phase transition temperature and photoluminescence properties in low-dimensional molecular perovskite ferroelastic crystals
Zhang, Jia-Mei; Xu, Zhe-Kun; Qin, Yan; Li, Peng-Fei; Wang, Zhong-Xia; CrystEngComm 27 (2025) 1534–1540; doi:10.1039/D5CE00012B

data_7249941
_publ_section_title
;
 High phase transition temperature and photoluminescence properties in
 low-dimensional molecular perovskite ferroelastic crystals
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1534
_journal_page_last               1540
_journal_paper_doi               10.1039/D5CE00012B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         '0.5(Cl6 Mn2), C5 H10 N'
_chemical_formula_sum            'C5 H10 Cl3 Mn N'
_chemical_formula_weight         245.43
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2025-01-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-31 deposited with the CCDC.	2025-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6427(16)
_cell_length_b                   6.4940(8)
_cell_length_c                   10.999(2)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    428.00(10)
_cell_measurement_theta_max      58.1450
_cell_measurement_theta_min      4.9070
_cell_volume                     1045.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      428.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00 -43.00   0.50    0.50    --  -75.30 -15.00 150.00   50
  2  \w   -111.00 -42.00   0.50    0.50    --  -75.30  -6.00-146.00  138
  3  \w   -102.00 -77.00   0.50    0.50    --  -74.13  -6.00-146.00   50
  4  \w    -80.00 -31.00   0.50    0.50    --  -60.41  -6.00-146.00   98
  5  \w    -58.00 -32.00   0.50    0.50    --  -75.30 125.00  30.00   52
  6  \w    -56.00 -31.00   0.50    0.50    --  -75.30 125.00  90.00   50
  7  \w   -101.00 -72.00   0.50    0.50    --  -75.30 125.00  90.00   58
  8  \w   -102.00 -76.00   0.50    0.50    --  -75.30 125.00  30.00   52
  9  \w     25.00  53.00   0.50    0.50    --   60.23   6.00  29.00   56
 10  \w     39.00 116.00   0.50    0.50    --   74.99   6.00  29.00  154
 11  \w     61.00 102.00   0.50    0.50    --   60.23  30.00 120.00   82
 12  \w     67.00  93.00   0.50    0.50    --   60.23   6.00  29.00   52
 13  \w     67.00 108.00   0.50    0.50    --   60.23  30.00-120.00   82
 14  \w     11.00  37.00   0.50    0.50    --   60.23 -30.00-150.00   52
 15  \w     12.00  37.00   0.50    0.50    --   60.23 -30.00 -90.00   50
 16  \w     11.00  36.00   0.50    0.50    --   60.23 -30.00 -60.00   50
 17  \w     11.00  38.00   0.50    0.50    --   60.23 -30.00 -30.00   54
 18  \w     12.00  38.00   0.50    0.50    --   60.23 -30.00   0.00   52
 19  \w     36.00  70.00   0.50    0.50    --   75.12 -94.00 -60.00   68
 20  \w     78.00 104.00   0.50    0.50    --   74.99-125.00-180.00   52
 21  \w     37.00  66.00   0.50    0.50    --   74.99-125.00-180.00   58
 22  \w     36.00  83.00   0.50    0.50    --   74.99 -94.00-120.00   94
 23  \w     27.00  70.00   0.50    0.50    --   60.23 -94.00  30.00   86
 24  \w     35.00  66.00   0.50    0.50    --   74.99 -94.00   0.00   62
 25  \w     45.00  74.00   0.50    0.50    --   75.12 -94.00  30.00   58
 26  \w     29.00  67.00   0.50    0.50    --   60.23 -94.00  90.00   76
 27  \w     37.00  66.00   0.50    0.50    --   60.23 -94.00 150.00   58
 28  \w     23.00  68.00   0.50    0.50    --   60.23 -94.00 120.00   90
 29  \w     49.00  74.00   0.50    0.50    --   75.12 -94.00 -90.00   50
 30  \w     59.00  85.00   0.50    0.50    --   75.12 -94.00-180.00   52
 31  \w   -118.00 -81.00   0.50    0.50    --  -74.13-125.00-120.00   74
 32  \w   -118.00 -78.00   0.50    0.50    --  -74.13-125.00 -90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0134772000
_diffrn_orient_matrix_UB_12      0.0064024000
_diffrn_orient_matrix_UB_13      -0.1389012000
_diffrn_orient_matrix_UB_21      0.1041078000
_diffrn_orient_matrix_UB_22      -0.0153095000
_diffrn_orient_matrix_UB_23      0.0177836000
_diffrn_orient_matrix_UB_31      -0.0063734000
_diffrn_orient_matrix_UB_32      -0.2366183000
_diffrn_orient_matrix_UB_33      -0.0051094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1456
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6822
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.528
_diffrn_reflns_theta_max         66.528
_diffrn_reflns_theta_min         5.029
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prism
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1008
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.3271
_refine_ls_R_factor_gt           0.2541
_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^)+(0.0500P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3984
_refine_ls_wR_factor_ref         0.4352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                620
_reflns_number_total             1008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00012b2.cif
_cod_data_source_block           zjm-241004-428k_r
_cod_depositor_comments
'Adding full bibliography for 7249938--7249941.cif.'
_cod_database_code               7249941
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Mn Cl'
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.284
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 = N1-C2 = N1-C3
 1.53 with sigma of 0.02
 C2-C3
 2.35 with sigma of 0.05
 C1-C2
 2.35 with sigma of 0.05
 C3-C1
 2.35 with sigma of 0.05
 C4-C3
 1.45 with sigma of 0.03
 C5-C4
 1.15 with sigma of 0.02
 C3-C5
 2.6 with sigma of 0.02
 C4-N1
 2.45 with sigma of 0.05
 C5-N1
 3.45 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
N1 \\sim C2 \\sim C3 \\sim C1 \\sim C4 \\sim C5: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: N1(0.5) H1(0.5) C2(0.5) H2a(0.5) H2b(0.5) H2c(0.5) C3(0.5)
 H3a(0.5) H3b(0.5) C4(0.5) C1(0.5) H1a(0.5) H1b(0.5) H1c(0.5) C5(0.5) H5(0.5)
5.a Riding coordinates:
 C2(H2a,H2b,H2c), C1(H1a,H1b,H1c)
5.b Ternary CH refined with riding coordinates:
 N1(H1)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b)
5.d :
 C5(H5)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.694
_oxdiff_exptl_absorpt_empirical_full_min 0.173