#------------------------------------------------------------------------------
#$Date: 2019-11-10 21:06:40 +0200 (Sun, 10 Nov 2019) $
#$Revision: 226190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/62/4516203.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_4516203
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             2018-09-25
_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                   8.477(4)
_cell_length_b                   9.052(4)
_cell_length_c                   26.186(11)
_cell_measurement_reflns_used    6645
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.85
_cell_volume                     2009.4(15)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      109.05
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.909
_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  0.1811
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10524
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.009
_diffrn_reflns_theta_min         2.863
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.525
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1512 before and 0.0849 after correction.
The Ratio of minimum to maximum transmission is 0.4897.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_refine_diff_density_max         3.003
_refine_diff_density_min         -2.724
_refine_diff_density_rms         0.545
_refine_ls_extinction_coef       0.0004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0789
_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)+(0.1075P)²+64.6701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1473
_reflns_number_total             1801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nz8b02349_si_007.cif
_cod_data_source_block           mo_sumitmatsc240918_0m
_cod_original_formula_sum        'C4 H12 I2 N Pb0.50'
_cod_database_code               4516203
_shelxl_version_number           2014-3
_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(I03) = Uanis(I02)
Uanis(C007) = Uanis(C1)
3.a Secondary CH2 refined with riding coordinates:
 C005(H00D,H00E), C006(H00F,H00G), C1(H1A,H1B)
3.b Idealised Me refined as rotating group:
 N004(H00A,H00B,H00C), C007(H00H,H00I,H00J)
;
_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 0.0000 0.5000 0.5000 0.0200(4) Uani 1 2 d S T P
I02 I 0.30337(14) 0.70247(14) 0.47678(4) 0.0253(4) Uani 1 1 d . . .
I03 I 0.07788(15) 0.47050(14) 0.61865(5) 0.0253(4) Uani 1 1 d . . .
N004 N 0.4849(19) 0.574(2) 0.5981(7) 0.032(4) Uani 1 1 d . . .
H00A H 0.5087 0.5032 0.5746 0.039 Uiso 1 1 calc GR . .
H00B H 0.5015 0.6648 0.5843 0.039 Uiso 1 1 calc GR . .
H00C H 0.3819 0.5651 0.6074 0.039 Uiso 1 1 calc GR . .
C005 C 0.585(2) 0.555(2) 0.6426(7) 0.023(4) Uani 1 1 d . . .
H00D H 0.5682 0.6395 0.6662 0.027 Uiso 1 1 calc R . .
H00E H 0.6966 0.5558 0.6319 0.027 Uiso 1 1 calc R . .
C006 C 0.549(2) 0.413(3) 0.6702(8) 0.029(4) Uani 1 1 d . . .
H00F H 0.4380 0.4153 0.6818 0.035 Uiso 1 1 calc R . .
H00G H 0.5597 0.3302 0.6457 0.035 Uiso 1 1 calc R . .
C007 C 0.608(3) 0.235(2) 0.7430(8) 0.033(3) Uani 1 1 d . . .
H00H H 0.6269 0.1514 0.7199 0.049 Uiso 1 1 calc GR . .
H00I H 0.4960 0.2373 0.7524 0.049 Uiso 1 1 calc GR . .
H00J H 0.6721 0.2230 0.7738 0.049 Uiso 1 1 calc GR . .
C1 C 0.653(3) 0.382(2) 0.7155(8) 0.033(3) Uani 1 1 d . . .
H1A H 0.6445 0.4652 0.7401 0.039 Uiso 1 1 calc R . .
H1B H 0.7645 0.3768 0.7041 0.039 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'
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_566
I02 Pb01 I02 91.54(3) 5_566 4_466
I02 Pb01 I02 88.45(3) . 4_466
I02 Pb01 I02 91.55(3) . 8_655
I02 Pb01 I02 180.00(4) 4_466 8_655
I02 Pb01 I02 88.46(3) 5_566 8_655
I03 Pb01 I02 86.19(3) . 5_566
I03 Pb01 I02 86.19(3) 5_566 .
I03 Pb01 I02 90.39(3) . 8_655
I03 Pb01 I02 93.81(3) 5_566 5_566
I03 Pb01 I02 93.81(3) . .
I03 Pb01 I02 89.61(3) . 4_466
I03 Pb01 I02 90.39(3) 5_566 4_466
I03 Pb01 I02 89.61(3) 5_566 8_655
I03 Pb01 I03 180.0 . 5_566
Pb01 I02 Pb01 148.60(4) . 4_566
H00A N004 H00B 109.5 . .
H00A N004 H00C 109.5 . .
H00B N004 H00C 109.5 . .
C005 N004 H00A 109.5 . .
C005 N004 H00B 109.5 . .
C005 N004 H00C 109.5 . .
N004 C005 H00D 109.3 . .
N004 C005 H00E 109.3 . .
N004 C005 C006 111.5(16) . .
H00D C005 H00E 108.0 . .
C006 C005 H00D 109.3 . .
C006 C005 H00E 109.3 . .
C005 C006 H00F 108.6 . .
C005 C006 H00G 108.6 . .
H00F C006 H00G 107.6 . .
C1 C006 C005 114.6(18) . .
C1 C006 H00F 108.6 . .
C1 C006 H00G 108.6 . .
H00H C007 H00I 109.5 . .
H00H C007 H00J 109.5 . .
H00I C007 H00J 109.5 . .
C1 C007 H00H 109.5 . .
C1 C007 H00I 109.5 . .
C1 C007 H00J 109.5 . .
C006 C1 C007 112.0(19) . .
C006 C1 H1A 109.2 . .
C006 C1 H1B 109.2 . .
C007 C1 H1A 109.2 . .
C007 C1 H1B 109.2 . .
H1A C1 H1B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 I02 3.2251(16) 8_655
Pb01 I02 3.2251(16) 4_466
Pb01 I02 3.2160(16) 5_566
Pb01 I02 3.2160(16) .
Pb01 I03 3.1876(18) .
Pb01 I03 3.1876(18) 5_566
I02 Pb01 3.2251(16) 4_566
N004 H00A 0.9100 .
N004 H00B 0.9100 .
N004 H00C 0.9100 .
N004 C005 1.45(3) .
C005 H00D 0.9900 .
C005 H00E 0.9900 .
C005 C006 1.51(3) .
C006 H00F 0.9900 .
C006 H00G 0.9900 .
C006 C1 1.51(3) .
C007 H00H 0.9800 .
C007 H00I 0.9800 .
C007 H00J 0.9800 .
C007 C1 1.57(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
