#------------------------------------------------------------------------------
#$Date: 2019-11-10 21:06:12 +0200 (Sun, 10 Nov 2019) $
#$Revision: 226188 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/62/4516201.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_4516201
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         'Br2 Pb0.5, C4 H12 N'
_chemical_formula_sum            'C4 H12 Br2 N Pb0.5'
_chemical_formula_weight         337.56
_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             2018-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.235(2)
_cell_length_b                   8.120(2)
_cell_length_c                   27.528(7)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.96
_cell_volume                     1840.7(8)
_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      99.94
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0797
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12713
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.117
_diffrn_reflns_theta_max         25.117
_diffrn_reflns_theta_min         2.882
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.828
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1590 before and 0.1055 after correction.
The Ratio of minimum to maximum transmission is 0.4815.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_F_000             1232
_refine_diff_density_max         2.637
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.403
_refine_ls_extinction_coef       0.0008(2)
_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   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0392P)²+239.7885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1406
_reflns_number_total             1566
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nz8b02349_si_003.cif
_cod_data_source_block           mo_np130318_0m
_cod_original_cell_volume        1840.9(8)
_cod_original_formula_sum        'C4 H12 Br2 N Pb0.50'
_cod_database_code               4516201
_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.
;
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.359
_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.a Secondary CH2 refined with riding coordinates:
 C006(H00D,H00E), C007(H00F,H00G), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 N005(H00A,H00B,H00C), C008(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 0.000000 0.500000 0.500000 0.0164(5) Uani 1 2 d S T P
Br02 Br -0.0299(3) 0.4808(2) 0.39087(8) 0.0208(6) Uani 1 1 d . . .
Br03 Br 0.3094(3) 0.6895(3) 0.49869(9) 0.0221(6) Uani 1 1 d . . .
N005 N 0.577(2) 0.576(2) 0.4108(7) 0.024(4) Uani 1 1 d . . .
H00A H 0.679952 0.543524 0.404022 0.028 Uiso 1 1 calc GR . .
H00B H 0.558976 0.569620 0.443328 0.028 Uiso 1 1 calc GR . .
H00C H 0.562908 0.682384 0.400828 0.028 Uiso 1 1 calc GR . .
C006 C 0.459(3) 0.468(3) 0.3846(10) 0.034(6) Uani 1 1 d . . .
H00D H 0.347221 0.501769 0.393074 0.041 Uiso 1 1 calc R . .
H00E H 0.473904 0.352851 0.396031 0.041 Uiso 1 1 calc R . .
C007 C 0.364(3) 0.362(4) 0.3037(10) 0.037(7) Uani 1 1 d . . .
H00F H 0.251468 0.389730 0.313574 0.044 Uiso 1 1 calc R . .
H00G H 0.385145 0.246825 0.313321 0.044 Uiso 1 1 calc R . .
C008 C 0.378(4) 0.377(5) 0.2491(10) 0.053(9) Uani 1 1 d . . .
H00H H 0.368328 0.267400 0.234429 0.079 Uiso 1 1 calc GR . .
H00I H 0.483438 0.424748 0.240709 0.079 Uiso 1 1 calc GR . .
H00J H 0.290902 0.447976 0.236842 0.079 Uiso 1 1 calc GR . .
C1 C 0.478(2) 0.472(3) 0.3301(7) 0.015(4) Uiso 1 1 d . . .
H1A H 0.462027 0.586424 0.318788 0.017 Uiso 1 1 calc R . .
H1B H 0.590882 0.439583 0.321828 0.017 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'
Br Br -0.2901 2.4595 '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
Br02 Pb01 Br02 180.0 . 5_566
Br03 Pb01 Br02 89.26(6) 4_466 5_566
Br03 Pb01 Br02 89.26(6) 8_655 .
Br03 Pb01 Br02 90.74(6) 4_466 .
Br03 Pb01 Br02 85.16(6) . 5_566
Br03 Pb01 Br02 94.84(6) 5_566 5_566
Br03 Pb01 Br02 94.84(6) . .
Br03 Pb01 Br02 90.74(6) 8_655 5_566
Br03 Pb01 Br02 85.16(6) 5_566 .
Br03 Pb01 Br03 90.79(3) 8_655 5_566
Br03 Pb01 Br03 89.21(3) 8_655 .
Br03 Pb01 Br03 90.79(3) 4_466 .
Br03 Pb01 Br03 89.21(3) 4_466 5_566
Br03 Pb01 Br03 180.0 . 5_566
Br03 Pb01 Br03 180.0 8_655 4_466
Pb01 Br03 Pb01 152.99(8) 4_566 .
N005 C006 C1 113(2) . .
C1 C007 C008 113(2) . .
C007 C1 C006 114(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 Br02 3.018(2) 5_566
Pb01 Br02 3.018(2) .
Pb01 Br03 2.971(2) 8_655
Pb01 Br03 2.976(2) 5_566
Pb01 Br03 2.971(2) 4_466
Pb01 Br03 2.976(2) .
N005 C006 1.50(3) .
C006 C1 1.51(4) .
C007 C008 1.51(4) .
C007 C1 1.49(3) .
