#------------------------------------------------------------------------------
#$Date: 2019-11-10 21:07:07 +0200 (Sun, 10 Nov 2019) $
#$Revision: 226192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/62/4516205.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_4516205
loop_
_publ_author_name
'Dutta, Sumit Kumar'
'Dutta, Anirban'
'Das Adhikari, Samrat'
'Pradhan, Narayan'
_publ_section_title
;
 Doping Mn2+ in Single-Crystalline Layered Perovskite Microcrystals
;
_journal_issue                   1
_journal_name_full               'ACS Energy Letters'
_journal_page_first              343
_journal_paper_doi               10.1021/acsenergylett.8b02349
_journal_volume                  4
_journal_year                    2018
_chemical_formula_moiety         'I2 Pb0.5, C4 H12 N'
_chemical_formula_sum            'C4 H12 I2 N Pb0.5'
_chemical_formula_weight         431.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.396(3)
_cell_length_b                   8.966(3)
_cell_length_c                   26.188(8)
_cell_measurement_reflns_used    7479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      3.11
_cell_volume                     1971.4(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.09
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13767
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.202
_diffrn_reflns_theta_min         2.882
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.806
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3780
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1664 before and 0.1008 after correction.
The Ratio of minimum to maximum transmission is 0.5072.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_F_000             1520
_refine_diff_density_max         4.245
_refine_diff_density_min         -4.663
_refine_diff_density_rms         0.622
_refine_ls_extinction_coef       0.00012(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.397
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.1123
_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/[σ²(Fo²)+(0.0001P)²+732.7255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2858
_refine_ls_wR_factor_ref         0.2913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1639
_reflns_number_total             1884
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nz8b02349_si_004.cif
_cod_data_source_block           mo_npmatsc130618_0m
_cod_original_cell_volume        1971.2(10)
_cod_original_formula_sum        'C4 H12 I2 N Pb0.50'
_cod_database_code               4516205
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C007) = Uanis(C008)
Uanis(C006) = Uanis(C005)
3.a Secondary CH2 refined with riding coordinates:
 C005(H00D,H00E), C006(H00F,H00G), C007(H00H,H00I)
3.b Idealised Me refined as rotating group:
 N004(H00A,H00B,H00C), C008(H00J,H00K,H00L)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
Pb01 Pb 0.500000 0.500000 0.500000 0.0186(6) Uani 1 2 d S T P
I02 I 0.8031(3) 0.2975(3) 0.52326(10) 0.0216(7) Uani 1 1 d . . .
I03 I 0.4216(3) 0.4704(3) 0.61872(10) 0.0227(7) Uani 1 1 d . . .
N004 N 0.017(5) 0.576(3) 0.5979(14) 0.028(8) Uani 1 1 d . . .
H00A H -0.014374 0.511348 0.573031 0.034 Uiso 1 1 calc GR . .
H00B H 0.119372 0.555137 0.607040 0.034 Uiso 1 1 calc GR . .
H00C H 0.011313 0.670976 0.585898 0.034 Uiso 1 1 calc GR . .
C005 C -0.047(5) 0.414(4) 0.6688(16) 0.019(6) Uani 1 1 d . . .
H00D H 0.065517 0.416110 0.680248 0.023 Uiso 1 1 calc R . .
H00E H -0.058417 0.330592 0.644310 0.023 Uiso 1 1 calc R . .
C006 C -0.085(5) 0.560(4) 0.6415(16) 0.019(6) Uani 1 1 d . . .
H00F H -0.197694 0.560556 0.630471 0.023 Uiso 1 1 calc R . .
H00G H -0.068509 0.645172 0.665094 0.023 Uiso 1 1 calc R . .
C007 C -0.155(6) 0.383(4) 0.7156(17) 0.031(8) Uani 1 1 d . . .
H00H H -0.144589 0.467477 0.739938 0.037 Uiso 1 1 calc R . .
H00I H -0.267196 0.379804 0.704149 0.037 Uiso 1 1 calc R . .
C008 C -0.116(6) 0.238(4) 0.7436(17) 0.031(8) Uani 1 1 d . . .
H00J H -0.137544 0.152914 0.721080 0.047 Uiso 1 1 calc GR . .
H00K H -0.181144 0.229867 0.774418 0.047 Uiso 1 1 calc GR . .
H00L H -0.002649 0.237395 0.753136 0.047 Uiso 1 1 calc GR . .
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'
I I -0.4742 1.8119 '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
I02 Pb01 I02 180.0 . 5_666
I02 Pb01 I02 88.51(3) 5_666 8_765
I02 Pb01 I02 91.49(3) . 8_765
I02 Pb01 I02 88.51(3) . 4_456
I02 Pb01 I02 180.00(9) 4_456 8_765
I02 Pb01 I02 91.49(3) 5_666 4_456
I02 Pb01 I03 93.95(7) 5_666 .
I02 Pb01 I03 86.05(7) . .
I02 Pb01 I03 93.95(7) . 5_666
I02 Pb01 I03 86.05(7) 5_666 5_666
I03 Pb01 I02 89.46(7) . 8_765
I03 Pb01 I02 90.54(7) . 4_456
I03 Pb01 I02 90.54(7) 5_666 8_765
I03 Pb01 I02 89.46(7) 5_666 4_456
I03 Pb01 I03 180.0 . 5_666
Pb01 I02 Pb01 148.48(9) . 4_556
C006 C005 C007 114(3) . .
N004 C006 C005 109(3) . .
C008 C007 C005 114(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 I02 3.185(3) .
Pb01 I02 3.197(3) 4_456
Pb01 I02 3.185(3) 5_666
Pb01 I02 3.197(3) 8_765
Pb01 I03 3.189(3) 5_666
Pb01 I03 3.189(3) .
N004 C006 1.44(5) .
C005 C006 1.53(5) .
C005 C007 1.55(6) .
C007 C008 1.53(6) .
