Dielectric phase transition of an A<sub>2</sub>BX<sub>4</sub>-type perovskite with a pentahedral to octahedral transformation.
Chai, Siqian; Xiong, Jianbo; Zheng, Yongshen; Shi, Rongchao; Xu, Jialiang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2218–2224; doi:10.1039/c9dt04270a

data_7703296
_publ_section_title
;
 Dielectric phase transition of an A<sub>2</sub>BX<sub>4</sub>-type
 perovskite with a pentahedral to octahedral transformation.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2218
_journal_page_last               2224
_journal_paper_doi               10.1039/c9dt04270a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(Cl16 Pb4), 4(C5 H12 N)'
_chemical_formula_sum            'C20 H48 Cl8 N4 Pb2'
_chemical_formula_weight         1042.60
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4936(8)
_cell_length_b                   23.8631(10)
_cell_length_c                   6.1802(2)
_cell_measurement_reflns_used    10035
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      30.0200
_cell_measurement_theta_min      3.3690
_cell_volume                     3317.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_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     -9.00  30.00   0.50    2.11    --    0.00 -57.00 120.00   78
  2  \w    -30.00  18.00   0.50    2.11    --    0.00 -77.00-150.00   96
  3  \w    -25.00  88.00   0.50    2.11    --    0.00  57.00-150.00  226
  4  \w    -19.00   6.00   0.50    2.11    --    0.00 -77.00-120.00   50
  5  \w     37.00  64.00   0.50    2.11    --    0.00  38.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170277000
_diffrn_orient_matrix_UB_12      -0.0250172000
_diffrn_orient_matrix_UB_13      -0.0035790000
_diffrn_orient_matrix_UB_21      0.0265146000
_diffrn_orient_matrix_UB_22      0.0159651000
_diffrn_orient_matrix_UB_23      0.0073336000
_diffrn_orient_matrix_UB_31      -0.0011679000
_diffrn_orient_matrix_UB_32      -0.0018100000
_diffrn_orient_matrix_UB_33      0.1144795000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            31870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.760
_diffrn_reflns_theta_min         2.489
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    10.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3861
_reflns_number_total             4528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04270a2.cif
_cod_data_source_block           csq-py-ysyz
_cod_depositor_comments
'Adding full bibliography for 7703293--7703296.cif.'
_cod_database_code               7703296
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Rigid bond restraints
 N6, C7, C8, C9, C10, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
N6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C2: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1AA(H1AA,H1AB), C2(H2A,H2B), C9(H9A,H9B), N4(H4A,H4B),
 C0AA(H0AA,H0AB), C1(H1A,H1B), C5(H5A,H5B), C3(H3A,H3B), C10(H10A,H10B), C7(H7A,
 H7B), N6(H6A,H6B)
;
_shelx_res_checksum              18228
_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 1.766
_oxdiff_exptl_absorpt_empirical_full_min 0.748