#------------------------------------------------------------------------------
#$Date: 2020-03-05 02:14:33 +0200 (Thu, 05 Mar 2020) $
#$Revision: 248968 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/32/7703296.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7703296
loop_
_publ_author_name
'Chai, Siqian'
'Xiong, Jianbo'
'Zheng, Yongshen'
'Shi, Rongchao'
'Xu, Jialiang'
_publ_section_title
;
 Dielectric phase transition of an A₂BX₄-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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  30.00   0.50    2.11    --    0.00 -57.00 120.00   78
  2  ω    -30.00  18.00   0.50    2.11    --    0.00 -77.00-150.00   96
  3  ω    -25.00  88.00   0.50    2.11    --    0.00  57.00-150.00  226
  4  ω    -19.00   6.00   0.50    2.11    --    0.00 -77.00-120.00   50
  5  ω     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       'ω 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/[σ²(Fo²)+(0.0328P)²] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb0A Pb 0.17405(2) 0.750000 0.37919(2) 0.00961(5) Uani 1 2 d S T P
Pb1A Pb 0.42445(2) 0.750000 0.24352(2) 0.00979(5) Uani 1 2 d S T P
Cl5 Cl 0.43416(3) 0.63065(3) 0.20596(12) 0.01466(15) Uani 1 1 d . . .
Cl4 Cl 0.39274(5) 0.750000 -0.16590(17) 0.0169(2) Uani 1 2 d S T P
Cl1 Cl 0.18162(5) 0.750000 0.81136(17) 0.0152(2) Uani 1 2 d S T P
Cl6 Cl 0.54471(4) 0.750000 0.11659(16) 0.0138(2) Uani 1 2 d S T P
Cl3 Cl 0.29778(4) 0.750000 0.36206(17) 0.0144(2) Uani 1 2 d S T P
C8 C 0.32588(17) 0.55914(16) 0.6472(6) 0.0245(8) Uani 1 1 d . U .
H8A H 0.359118 0.539908 0.580188 0.029 Uiso 1 1 calc R . .
H8B H 0.290581 0.551411 0.562057 0.029 Uiso 1 1 calc R . .
C1AA C 0.57085(15) 0.56621(14) 0.4858(5) 0.0176(7) Uani 1 1 d . . .
H1AA H 0.532004 0.557955 0.425492 0.021 Uiso 1 1 calc R . .
H1AB H 0.600727 0.552185 0.386408 0.021 Uiso 1 1 calc R . .
C2 C 0.27724(15) 0.63102(14) 0.9847(5) 0.0180(7) Uani 1 1 d . U .
H2A H 0.243157 0.650179 1.046089 0.022 Uiso 1 1 calc R . .
H2B H 0.311584 0.639233 1.074156 0.022 Uiso 1 1 calc R . .
C9 C 0.31711(16) 0.53705(16) 0.8771(6) 0.0226(8) Uani 1 1 d . U .
H9A H 0.308241 0.497281 0.872941 0.027 Uiso 1 1 calc R . .
H9B H 0.353251 0.542339 0.960220 0.027 Uiso 1 1 calc R . .
N4 N 0.54194(12) 0.62317(12) 0.8876(4) 0.0134(5) Uani 1 1 d . . .
H4A H 0.578067 0.630355 0.939372 0.016 Uiso 1 1 calc R . .
H4B H 0.515532 0.636375 0.981962 0.016 Uiso 1 1 calc R . .
C0AA C 0.57748(15) 0.53700(15) 0.7045(5) 0.0180(7) Uani 1 1 d . . .
H0AA H 0.569967 0.497211 0.687627 0.022 Uiso 1 1 calc R . .
H0AB H 0.617833 0.541634 0.756853 0.022 Uiso 1 1 calc R . .
C1 C 0.57795(14) 0.62968(14) 0.5116(5) 0.0152(6) Uani 1 1 d . . .
H1A H 0.618215 0.638015 0.557747 0.018 Uiso 1 1 calc R . .
H1B H 0.571483 0.647717 0.372978 0.018 Uiso 1 1 calc R . .
C5 C 0.53431(15) 0.65310(14) 0.6762(5) 0.0170(6) Uani 1 1 d . . .
H5A H 0.541362 0.692879 0.695887 0.020 Uiso 1 1 calc R . .
H5B H 0.493960 0.648188 0.624206 0.020 Uiso 1 1 calc R . .
C3 C 0.53423(15) 0.56132(14) 0.8680(5) 0.0183(7) Uani 1 1 d . . .
H3A H 0.493833 0.553074 0.823200 0.022 Uiso 1 1 calc R . .
H3B H 0.540760 0.543948 1.007895 0.022 Uiso 1 1 calc R . .
C10 C 0.26605(16) 0.56858(15) 0.9832(6) 0.0232(7) Uani 1 1 d . U .
H10A H 0.229515 0.560854 0.905343 0.028 Uiso 1 1 calc R . .
H10B H 0.261146 0.555464 1.130726 0.028 Uiso 1 1 calc R . .
C7 C 0.33766(15) 0.62164(15) 0.6483(6) 0.0210(7) Uani 1 1 d . U .
H7A H 0.374763 0.629212 0.722799 0.025 Uiso 1 1 calc R . .
H7B H 0.341310 0.635095 0.500813 0.025 Uiso 1 1 calc R . .
Cl2 Cl 0.17680(3) 0.63029(3) 0.43939(13) 0.01357(15) Uani 1 1 d . . .
N6 N 0.28794(12) 0.65171(12) 0.7595(4) 0.0135(5) Uani 1 1 d . U .
H6A H 0.254820 0.647476 0.682398 0.016 Uiso 1 1 calc R . .
H6B H 0.296305 0.688144 0.764217 0.016 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Pb0A Cl6 93.13(3) . 6_556
Cl1 Pb0A Cl3 88.53(3) . .
Cl1 Pb0A Cl2 82.516(16) . 8_575
Cl1 Pb0A Cl2 82.517(16) . .
Cl3 Pb0A Cl6 178.34(3) . 6_556
Cl3 Pb0A Cl2 89.055(14) . .
Cl3 Pb0A Cl2 89.053(14) . 8_575
Cl2 Pb0A Cl6 91.163(14) 8_575 6_556
Cl2 Pb0A Cl6 91.161(14) . 6_556
Cl2 Pb0A Cl2 164.96(3) . 8_575
Cl5 Pb1A Cl5 167.23(3) 8_575 .
Cl5 Pb1A Cl3 95.395(15) 8_575 .
Cl5 Pb1A Cl3 95.396(15) . .
Cl4 Pb1A Cl5 86.717(16) . .
Cl4 Pb1A Cl5 86.717(16) . 8_575
Cl4 Pb1A Cl6 89.57(3) . .
Cl4 Pb1A Cl3 88.68(3) . .
Cl6 Pb1A Cl5 84.503(15) . 8_575
Cl6 Pb1A Cl5 84.502(15) . .
Cl6 Pb1A Cl3 178.25(3) . .
Pb1A Cl6 Pb0A 163.31(4) . 6_656
Pb0A Cl3 Pb1A 167.76(4) . .
C7 C8 C9 111.0(3) . .
C0AA C1AA C1 110.4(3) . .
N6 C2 C10 110.3(3) . .
C10 C9 C8 109.1(3) . .
C3 N4 C5 112.8(2) . .
C3 C0AA C1AA 110.6(3) . .
C5 C1 C1AA 111.5(3) . .
N4 C5 C1 109.5(3) . .
N4 C3 C0AA 111.0(3) . .
C2 C10 C9 111.4(3) . .
N6 C7 C8 110.1(3) . .
C7 N6 C2 112.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb0A Cl1 2.6763(11) .
Pb0A Cl6 2.9095(10) 6_556
Pb0A Cl3 2.7851(10) .
Pb0A Cl2 2.8814(8) .
Pb0A Cl2 2.8815(8) 8_575
Pb1A Cl5 2.8657(8) 8_575
Pb1A Cl5 2.8658(8) .
Pb1A Cl4 2.6289(11) .
Pb1A Cl6 2.8166(10) .
Pb1A Cl3 2.9418(10) .
C8 C9 1.528(5) .
C8 C7 1.515(5) .
C1AA C0AA 1.528(5) .
C1AA C1 1.531(5) .
C2 C10 1.511(5) .
C2 N6 1.496(4) .
C9 C10 1.522(5) .
N4 C5 1.499(4) .
N4 C3 1.491(4) .
C0AA C3 1.518(5) .
C1 C5 1.520(4) .
C7 N6 1.496(4) .
