Post-synthetic halide conversion and selective halogen capture in hybrid perovskites
Solis-Ibarra, D.; Smith, I. C.; Karunadasa, H. I.; Chem. Sci. 6 (2015) 4054–; doi:10.1039/C5SC01135C

data_1519437
_publ_section_title
;
 Post-synthetic halide conversion and selective halogen capture in hybrid
 perovskites
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4054
_journal_paper_doi               10.1039/C5SC01135C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'Cl4 Pb, 2(C4 H10 Br2 N)'
_chemical_formula_sum            'C8 H20 Br4 Cl4 N2 Pb'
_chemical_formula_weight         812.89
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3655(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4158(7)
_cell_length_b                   5.4438(7)
_cell_length_c                   35.809(4)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      3.65
_cell_volume                     1053.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ALS Beamline 11.3.1'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.68880
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            25379
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.797
_exptl_absorpt_correction_T_max  0.4928
_exptl_absorpt_correction_T_min  0.3004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1259 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.6096.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.843
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+21.5615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                2709
_reflns_number_total             2736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01135c3.cif
_cod_data_source_block           ds167-final
_cod_depositor_comments
'Adding full bibliography for 1519436--1519438.cif.'
_cod_database_code               1519437
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 C3-Br1 \\sim C3A-Br1
 with sigma of 0.02
 C4-Br2 \\sim C4A-Br2
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Same fragment restrains
{N1, C1, C2, C3, C4}
as
{N1A, C1A, C2A, C3A, C4A}
6. Others
 Sof(Cl3B)=1-FVAR(1)
 Sof(Cl3A)=FVAR(1)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C1)=Sof(H1D)=Sof(H1E)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
 Fixed Sof: Cl1(0.5) Cl2(0.5)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C3A(H3A)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C4(H4A,H4B), C1A(H1AD,H1AE), C2A(H2AA,H2AB),
 C4A(H4AA,H4AB)
7.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N1A(H1AA,H1AB,H1AC)
;
_olex2_submission_special_instructions 'No special instructions were received'